
data_013rwfk20
_audit_creation_date               2020-11-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      '12 Mansfield Road, OX1 3TA'
_audit_contact_author_email        'Charlotte.Williams@chem.ox.ac.uk'
_audit_contact_author_name         'Charlotte Williams'
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           'C25 H30 Al N2 Na O8, 2(C H2 Cl2)'
_chemical_formula_sum              'C27 H34 Al Cl4 N2 Na O8'
_chemical_formula_weight           706.33
_chemical_melting_point            ?
_chemical_oxdiff_formula           C25H33Al1N2Na1O8
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Al' 'Al' 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Na' 'Na' 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        triclinic
_space_group_IT_number             2
_space_group_name_H-M_alt          'P -1'
_space_group_name_Hall             '-P 1'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                     10.7960(5)
_cell_length_b                     11.9409(8)
_cell_length_c                     14.6196(7)
_cell_angle_alpha                  66.034(5)
_cell_angle_beta                   84.098(4)
_cell_angle_gamma                  69.361(5)
_cell_volume                       1609.86(17)
_cell_formula_units_Z              2
_cell_measurement_reflns_used      4582
_cell_measurement_temperature      150.01(10)
_cell_measurement_theta_max        76.2360
_cell_measurement_theta_min        3.3100
_shelx_estimated_absorpt_T_max     0.812
_shelx_estimated_absorpt_T_min     0.534
_exptl_absorpt_coefficient_mu      4.168
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.89317
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              'clear yellowish black'
_exptl_crystal_colour_lustre       clear
_exptl_crystal_colour_modifier     yellowish
_exptl_crystal_colour_primary      black
_exptl_crystal_density_diffrn      1.457
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               732
_exptl_crystal_preparation         ?
_exptl_crystal_size_max            0.172
_exptl_crystal_size_mid            0.145
_exptl_crystal_size_min            0.052
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0313
_diffrn_reflns_av_unetI/netI       0.0431
_diffrn_reflns_Laue_measured_fraction_full  0.999
_diffrn_reflns_Laue_measured_fraction_max  0.986
_diffrn_reflns_limit_h_max         13
_diffrn_reflns_limit_h_min         -12
_diffrn_reflns_limit_k_max         15
_diffrn_reflns_limit_k_min         -14
_diffrn_reflns_limit_l_max         18
_diffrn_reflns_limit_l_min         -16
_diffrn_reflns_number              12886
_diffrn_reflns_point_group_measured_fraction_full  0.999
_diffrn_reflns_point_group_measured_fraction_max  0.986
_diffrn_reflns_theta_full          67.684
_diffrn_reflns_theta_max           76.512
_diffrn_reflns_theta_min           3.312
_diffrn_ambient_environment        N~2~
_diffrn_ambient_temperature        150.01(10)
_diffrn_detector                   'CCD plate'
_diffrn_detector_area_resol_mean   10.5035
_diffrn_detector_type              Atlas
_diffrn_measured_fraction_theta_full  0.999
_diffrn_measured_fraction_theta_max  0.986
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω     13.00  51.00   1.00    1.00    --    0.00 -99.00-150.00   38
  2  ω     14.00  44.00   1.00    1.00    --    0.00 -77.00  30.00   30
  3  ω    -21.00   6.00   1.00    1.00    --    0.00 -77.00  30.00   27
  4  ω     -5.00  36.00   1.00    1.00    --    0.00  19.00-150.00   41
  5  ω     56.00  83.00   1.00    1.00    --    0.00  19.00-150.00   27
  6  ω    -81.00   0.00   1.00    3.00    --  -60.50  77.00  90.00   81
  7  ω     15.00  40.00   1.00    3.00    --  -60.50  77.00  90.00   25
  8  ω    121.00 158.00   1.00    3.00    --   60.50  77.00 -30.00   37
  9  ω     97.00 122.00   1.00    3.00    --   60.50 125.00-180.00   25
 10  ω    101.00 152.00   1.00    3.00    --   60.50 125.00 -90.00   51
 11  ω    101.00 152.00   1.00    3.00    --   60.50 125.00  90.00   51
 12  ω    101.00 139.00   1.00    3.00    --   60.50 125.00  30.00   38
 13  ω    -31.00 152.00   1.00    3.00    --   60.50   0.00  30.00  183
 14  ω     27.00 112.00   1.00    3.00    --   60.50-125.00 -90.00   85
 15  ω    122.00 157.00   1.00    3.00    --   60.50  77.00 150.00   35
 16  ω     65.00  92.00   1.00    8.00    --  121.00 178.00   0.00   27
 17  ω     79.00 108.00   1.00    8.00    --  121.00-111.00 150.00   29
 18  ω     77.00 177.00   1.00    8.00    --  121.00  25.00 120.00  100
 19  ω     30.00  63.00   1.00    8.00    --  121.00 -37.00-120.00   33
 20  ω     29.00 108.00   1.00    8.00    --  121.00-111.00  90.00   79
 21  ω     45.00  70.00   1.00    8.00    --  121.00  25.00 120.00   25
 22  ω     30.00  85.00   1.00    8.00    --  121.00 -77.00   0.00   55
 23  ω     36.00 108.00   1.00    8.00    --  121.00-111.00   0.00   72
 24  ω     37.00  64.00   1.00    8.00    --  121.00 -37.00 -30.00   27
 25  ω     34.00  64.00   1.00    8.00    --  121.00 -37.00  90.00   30
 26  ω    108.00 178.00   1.00    8.00    --  121.00 111.00 -60.00   70
 27  ω     24.00 107.00   1.00    8.00    --  121.00 -91.00-150.00   83
 28  ω     62.00  92.00   1.00    8.00    --  121.00 -63.00  90.00   30
 29  ω     80.00 108.00   1.00    8.00    --  121.00-111.00-150.00   28
 30  ω     35.00 107.00   1.00    8.00    --  121.00-111.00 -60.00   72
 31  ω     30.00  55.00   1.00    8.00    --  121.00 -37.00 -90.00   25
 32  ω     81.00 178.00   1.00    8.00    --  121.00  50.00   0.00   97
 33  ω     40.00  80.00   1.00    8.00    --  121.00 -63.00-150.00   40
 34  ω     32.00  60.00   1.00    8.00    --  121.00 -37.00-150.00   28
 35  ω     35.00  78.00   1.00    8.00    --  121.00 -50.00  60.00   43
 36  ω     41.00  66.00   1.00    8.00    --  121.00 -50.00 120.00   25
 37  ω     56.00  87.00   1.00    8.00    --  121.00-111.00 -30.00   31
 38  ω     24.00  54.00   1.00    8.00    --  121.00 -91.00  60.00   30
 39  ω     82.00 107.00   1.00    8.00    --  121.00 -91.00  60.00   25
 40  ω     83.00 108.00   1.00    8.00    --  121.00-111.00  60.00   25
 41  ω     48.00  75.00   1.00    8.00    --  121.00  25.00-120.00   27
 42  ω    119.00 157.00   1.00    8.00    --  121.00  25.00-120.00   38
 43  ω     98.00 126.00   1.00    8.00    --  121.00 -77.00   0.00   28
;
_diffrn_measurement_device         'four-circle diffractometer'
_diffrn_measurement_device_type    'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_type        
 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11        0.0104115000
_diffrn_orient_matrix_UB_12        -0.1381687000
_diffrn_orient_matrix_UB_13        0.0142178000
_diffrn_orient_matrix_UB_21        0.1087122000
_diffrn_orient_matrix_UB_22        -0.0010036000
_diffrn_orient_matrix_UB_23        -0.0769710000
_diffrn_orient_matrix_UB_31        0.1066597000
_diffrn_orient_matrix_UB_32        -0.0589934000
_diffrn_orient_matrix_UB_33        0.0848618000
_diffrn_radiation_monochromator    mirror
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             CuK\a
_diffrn_radiation_wavelength       1.54184
_diffrn_source                     'micro-focus sealed X-ray tube'
_diffrn_source_type                'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  5365
_reflns_number_total               6670
_reflns_odcompleteness_completeness  99.71
_reflns_odcompleteness_iscentric   1
_reflns_odcompleteness_theta       74.33
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection         'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction          'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.496
_refine_diff_density_min           -0.345
_refine_diff_density_rms           0.057
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.033
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       404
_refine_ls_number_reflns           6670
_refine_ls_number_restraints       1
_refine_ls_R_factor_all            0.0554
_refine_ls_R_factor_gt             0.0425
_refine_ls_restrained_S_all        1.051
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0619P)²+0.3016P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1105
_refine_ls_wR_factor_ref           0.1210
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl2S-C1S \\sim Cl3S-C1S
 with sigma of 0.02
3. Others
 Sof(H1SC)=Sof(H1SD)=Sof(Cl3S)=1-FVAR(1)
 Sof(Cl2S)=Sof(H1SA)=Sof(H1SB)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C13(H13A,H13B), C2S(H2SA,H2SB), C1S(H1SA,H1SB), C1S(H1SC,H1SD)
4.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C8(H8), C17(H17), C16(H16), C18(H18), C3(H3), C4(H4), C5(H5)
4.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C), C21(H21A,H21B,H21C), C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Al1 Al 0.62253(5) 0.40762(5) 0.29802(4) 0.02446(13) Uani 1 1 d . . . . .
 Na1 Na 0.42987(8) 0.43534(8) -0.05414(6) 0.03110(18) Uani 1 1 d . . . . .
 O2 O 0.72571(13) 0.41750(14) 0.18781(10) 0.0284(3) Uani 1 1 d . . . . .
 O3 O 0.50141(13) 0.56261(13) 0.21432(10) 0.0272(3) Uani 1 1 d . . . . .
 O7 O 0.69800(14) 0.49045(15) 0.34915(11) 0.0312(3) Uani 1 1 d . . . . .
 O5 O 0.54277(14) 0.30462(14) 0.27183(10) 0.0283(3) Uani 1 1 d . . . . .
 O4 O 0.37022(15) 0.75285(15) 0.05250(11) 0.0344(3) Uani 1 1 d . . . . .
 O6 O 0.49326(16) 0.38216(15) 0.10745(11) 0.0348(3) Uani 1 1 d . . . . .
 O1 O 0.80293(16) 0.48474(16) 0.00417(11) 0.0373(3) Uani 1 1 d . . . . .
 O8 O 0.84815(17) 0.5081(2) 0.42833(12) 0.0447(4) Uani 1 1 d . . . . .
 N2 N 0.49900(16) 0.39959(16) 0.41367(12) 0.0251(3) Uani 1 1 d . . . . .
 N1 N 0.76215(16) 0.23298(17) 0.38372(13) 0.0288(3) Uani 1 1 d . . . . .
 C20 C 0.37243(19) 0.61253(18) 0.22057(14) 0.0255(4) Uani 1 1 d . . . . .
 C14 C 0.37476(19) 0.46942(19) 0.40177(14) 0.0267(4) Uani 1 1 d . . . . .
 H14 H 0.325196 0.454452 0.458652 0.032 Uiso 1 1 calc R . . . .
 C7 C 0.82165(19) 0.3277(2) 0.16799(15) 0.0293(4) Uani 1 1 d . . . . .
 C15 C 0.30478(19) 0.56887(19) 0.30856(15) 0.0272(4) Uani 1 1 d . . . . .
 C24 C 0.8092(2) 0.5037(2) 0.35406(15) 0.0295(4) Uani 1 1 d . . . . .
 C22 C 0.4989(2) 0.3021(2) 0.19513(15) 0.0293(4) Uani 1 1 d . . . . .
 C19 C 0.2967(2) 0.7185(2) 0.13555(15) 0.0289(4) Uani 1 1 d . . . . .
 C10 C 0.6375(2) 0.1825(2) 0.54395(14) 0.0295(4) Uani 1 1 d . . . . .
 C6 C 0.8846(2) 0.2013(2) 0.24007(16) 0.0321(4) Uani 1 1 d . . . . .
 C8 C 0.8545(2) 0.1657(2) 0.34484(16) 0.0328(4) Uani 1 1 d . . . . .
 H8 H 0.908230 0.084644 0.389140 0.039 Uiso 1 1 calc R . . . .
 C2 C 0.8686(2) 0.3593(2) 0.06919(16) 0.0322(4) Uani 1 1 d . . . . .
 C17 C 0.0974(2) 0.7349(2) 0.22786(17) 0.0362(4) Uani 1 1 d . . . . .
 H17 H 0.006857 0.775626 0.230213 0.043 Uiso 1 1 calc R . . . .
 C9 C 0.7693(2) 0.1794(2) 0.49456(15) 0.0326(4) Uani 1 1 d . . . . .
 H9A H 0.807411 0.228027 0.515580 0.039 Uiso 1 1 calc R . . . .
 H9B H 0.829126 0.089677 0.519104 0.039 Uiso 1 1 calc R . . . .
 C13 C 0.5471(2) 0.3236(2) 0.51959(14) 0.0306(4) Uani 1 1 d . . . . .
 H13A H 0.471141 0.322976 0.561186 0.037 Uiso 1 1 calc R . . . .
 H13B H 0.594971 0.367644 0.537381 0.037 Uiso 1 1 calc R . . . .
 C16 C 0.1672(2) 0.6321(2) 0.31109(17) 0.0340(4) Uani 1 1 d . . . . .
 H16 H 0.123606 0.603640 0.369740 0.041 Uiso 1 1 calc R . . . .
 C18 C 0.1622(2) 0.7790(2) 0.13922(17) 0.0335(4) Uani 1 1 d . . . . .
 H18 H 0.114613 0.848864 0.082886 0.040 Uiso 1 1 calc R . . . .
 C11 C 0.5689(2) 0.1084(2) 0.51488(16) 0.0355(4) Uani 1 1 d . . . . .
 H11A H 0.550151 0.148165 0.443773 0.053 Uiso 1 1 calc GR . . . .
 H11B H 0.487652 0.111119 0.548892 0.053 Uiso 1 1 calc GR . . . .
 H11C H 0.626017 0.019283 0.533733 0.053 Uiso 1 1 calc GR . . . .
 C12 C 0.6683(2) 0.1188(2) 0.65804(15) 0.0375(5) Uani 1 1 d . . . . .
 H12A H 0.726384 0.030121 0.676781 0.056 Uiso 1 1 calc GR . . . .
 H12B H 0.587288 0.120461 0.692341 0.056 Uiso 1 1 calc GR . . . .
 H12C H 0.710247 0.166197 0.676062 0.056 Uiso 1 1 calc GR . . . .
 C3 C 0.9728(2) 0.2694(3) 0.04551(18) 0.0400(5) Uani 1 1 d . . . . .
 H3 H 1.003312 0.292579 -0.019077 0.048 Uiso 1 1 calc R . . . .
 C23 C 0.4520(3) 0.1878(2) 0.21968(17) 0.0422(5) Uani 1 1 d . . . . .
 H23A H 0.525539 0.107780 0.245925 0.063 Uiso 1 1 calc GR . . . .
 H23B H 0.414914 0.194502 0.159964 0.063 Uiso 1 1 calc GR . . . .
 H23C H 0.385673 0.188949 0.268713 0.063 Uiso 1 1 calc GR . . . .
 C4 C 1.0324(2) 0.1443(3) 0.1175(2) 0.0436(5) Uani 1 1 d . . . . .
 H4 H 1.101525 0.083919 0.100659 0.052 Uiso 1 1 calc R . . . .
 C25 C 0.8951(2) 0.5158(3) 0.26454(18) 0.0404(5) Uani 1 1 d . . . . .
 H25A H 0.939705 0.431090 0.263599 0.061 Uiso 1 1 calc GR . . . .
 H25B H 0.959364 0.552266 0.268994 0.061 Uiso 1 1 calc GR . . . .
 H25C H 0.840629 0.571673 0.204150 0.061 Uiso 1 1 calc GR . . . .
 C21 C 0.3017(3) 0.8633(2) -0.03391(17) 0.0424(5) Uani 1 1 d . . . . .
 H21A H 0.363438 0.882695 -0.084968 0.064 Uiso 1 1 calc GR . . . .
 H21B H 0.259984 0.936948 -0.016449 0.064 Uiso 1 1 calc GR . . . .
 H21C H 0.235474 0.844478 -0.058487 0.064 Uiso 1 1 calc GR . . . .
 C5 C 0.9889(2) 0.1098(2) 0.21393(19) 0.0411(5) Uani 1 1 d . . . . .
 H5 H 1.028462 0.025948 0.261796 0.049 Uiso 1 1 calc R . . . .
 C1 C 0.8507(3) 0.5259(3) -0.09506(17) 0.0444(5) Uani 1 1 d . . . . .
 H1A H 0.840385 0.474029 -0.127650 0.067 Uiso 1 1 calc GR . . . .
 H1B H 0.942698 0.515093 -0.091281 0.067 Uiso 1 1 calc GR . . . .
 H1C H 0.800971 0.616010 -0.132666 0.067 Uiso 1 1 calc GR . . . .
 Cl5S Cl 0.68129(6) 0.83966(6) 0.22178(4) 0.04518(14) Uani 1 1 d . . . . .
 Cl4S Cl 0.66452(7) 0.81475(8) 0.03262(5) 0.05499(17) Uani 1 1 d . . . . .
 C2S C 0.5845(3) 0.8179(3) 0.1442(2) 0.0454(5) Uani 1 1 d . . . . .
 H2SA H 0.499765 0.888454 0.127137 0.054 Uiso 1 1 calc R . . . .
 H2SB H 0.567675 0.736733 0.180623 0.054 Uiso 1 1 calc R . . . .
 Cl1S Cl 0.85813(12) -0.14396(11) 0.39608(7) 0.0835(3) Uani 1 1 d . . . . .
 Cl2S Cl 0.7960(3) -0.2659(2) 0.60201(15) 0.0662(10) Uani 0.451(5) 1 d D . P A 1
 C1S C 0.8610(3) -0.2794(3) 0.5028(3) 0.0675(9) Uani 1 1 d D . . . .
 H1SA H 0.818992 -0.327544 0.484522 0.081 Uiso 0.451(5) 1 calc R . P A 1
 H1SB H 0.953160 -0.333939 0.520356 0.081 Uiso 0.451(5) 1 calc R . P A 1
 H1SC H 0.940233 -0.353083 0.508025 0.081 Uiso 0.549(5) 1 calc R . P A 2
 H1SD H 0.783734 -0.303266 0.503347 0.081 Uiso 0.549(5) 1 calc R . P A 2
 Cl3S Cl 0.8598(3) -0.2249(2) 0.60796(13) 0.0760(9) Uani 0.549(5) 1 d D . P A 2


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Al1 Na1 3.2840(10) 2_665 ?
 Al1 O2 1.8494(15) . ?
 Al1 O3 1.8481(15) . ?
 Al1 O7 1.8694(16) . ?
 Al1 O5 1.8967(15) . ?
 Al1 N2 2.0350(17) . ?
 Al1 N1 2.0592(18) . ?
 Na1 Na1 3.3630(17) 2_665 ?
 Na1 O2 2.3521(16) 2_665 ?
 Na1 O3 2.3756(15) 2_665 ?
 Na1 O4 2.5013(18) 2_665 ?
 Na1 O6 2.2934(16) . ?
 Na1 O6 2.4098(17) 2_665 ?
 Na1 O1 2.5018(17) 2_665 ?
 O2 C7 1.310(2) . ?
 O3 C20 1.317(2) . ?
 O7 C24 1.278(2) . ?
 O5 C22 1.277(2) . ?
 O4 C19 1.378(2) . ?
 O4 C21 1.426(2) . ?
 O6 C22 1.241(2) . ?
 O1 C2 1.372(3) . ?
 O1 C1 1.434(2) . ?
 O8 C24 1.230(3) . ?
 N2 C14 1.291(3) . ?
 N2 C13 1.477(2) . ?
 N1 C8 1.286(3) . ?
 N1 C9 1.480(2) . ?
 C20 C15 1.411(3) . ?
 C20 C19 1.420(3) . ?
 C14 C15 1.450(3) . ?
 C7 C6 1.407(3) . ?
 C7 C2 1.424(3) . ?
 C15 C16 1.414(3) . ?
 C24 C25 1.511(3) . ?
 C22 C23 1.516(3) . ?
 C19 C18 1.382(3) . ?
 C10 C9 1.523(3) . ?
 C10 C13 1.531(3) . ?
 C10 C11 1.531(3) . ?
 C10 C12 1.542(3) . ?
 C6 C8 1.448(3) . ?
 C6 C5 1.412(3) . ?
 C2 C3 1.382(3) . ?
 C17 C16 1.371(3) . ?
 C17 C18 1.401(3) . ?
 C3 C4 1.392(4) . ?
 C4 C5 1.380(3) . ?
 Cl5S C2S 1.766(3) . ?
 Cl4S C2S 1.774(3) . ?
 Cl1S C1S 1.725(4) . ?
 Cl2S C1S 1.589(4) . ?
 C1S Cl3S 1.895(4) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O2 Al1 Na1 44.44(5) . 2_665 ?
 O2 Al1 O7 96.96(7) . . ?
 O2 Al1 O5 91.97(7) . . ?
 O2 Al1 N2 176.38(7) . . ?
 O2 Al1 N1 90.35(7) . . ?
 O3 Al1 Na1 45.18(5) . 2_665 ?
 O3 Al1 O2 86.44(6) . . ?
 O3 Al1 O7 93.43(7) . . ?
 O3 Al1 O5 93.16(7) . . ?
 O3 Al1 N2 91.06(7) . . ?
 O3 Al1 N1 176.54(7) . . ?
 O7 Al1 Na1 110.35(5) . 2_665 ?
 O7 Al1 O5 169.21(7) . . ?
 O7 Al1 N2 85.79(7) . . ?
 O7 Al1 N1 88.22(7) . . ?
 O5 Al1 Na1 80.30(5) . 2_665 ?
 O5 Al1 N2 85.56(6) . . ?
 O5 Al1 N1 85.67(7) . . ?
 N2 Al1 Na1 132.32(5) . 2_665 ?
 N2 Al1 N1 92.10(7) . . ?
 N1 Al1 Na1 131.37(5) . 2_665 ?
 Al1 Na1 Na1 114.56(4) 2_665 2_665 ?
 O2 Na1 Al1 33.40(4) 2_665 2_665 ?
 O2 Na1 Na1 116.86(6) 2_665 2_665 ?
 O2 Na1 O3 64.76(5) 2_665 2_665 ?
 O2 Na1 O4 127.61(6) 2_665 2_665 ?
 O2 Na1 O6 81.23(6) 2_665 2_665 ?
 O2 Na1 O1 64.95(5) 2_665 2_665 ?
 O3 Na1 Al1 33.49(4) 2_665 2_665 ?
 O3 Na1 Na1 118.61(5) 2_665 2_665 ?
 O3 Na1 O4 64.69(5) 2_665 2_665 ?
 O3 Na1 O6 82.66(5) 2_665 2_665 ?
 O3 Na1 O1 126.84(6) 2_665 2_665 ?
 O4 Na1 Al1 98.16(4) 2_665 2_665 ?
 O4 Na1 Na1 98.64(5) 2_665 2_665 ?
 O4 Na1 O1 148.51(6) 2_665 2_665 ?
 O6 Na1 Al1 160.31(5) . 2_665 ?
 O6 Na1 Al1 71.58(4) 2_665 2_665 ?
 O6 Na1 Na1 45.76(4) . 2_665 ?
 O6 Na1 Na1 42.98(4) 2_665 2_665 ?
 O6 Na1 O2 145.34(7) . 2_665 ?
 O6 Na1 O3 146.76(7) . 2_665 ?
 O6 Na1 O4 105.03(6) 2_665 2_665 ?
 O6 Na1 O4 87.01(6) . 2_665 ?
 O6 Na1 O6 88.74(6) . 2_665 ?
 O6 Na1 O1 105.57(6) 2_665 2_665 ?
 O6 Na1 O1 86.40(6) . 2_665 ?
 O1 Na1 Al1 98.34(5) 2_665 2_665 ?
 O1 Na1 Na1 98.60(5) 2_665 2_665 ?
 Al1 O2 Na1 102.15(6) . 2_665 ?
 C7 O2 Al1 131.33(13) . . ?
 C7 O2 Na1 114.87(12) . 2_665 ?
 Al1 O3 Na1 101.33(6) . 2_665 ?
 C20 O3 Al1 129.98(12) . . ?
 C20 O3 Na1 114.79(12) . 2_665 ?
 C24 O7 Al1 139.93(14) . . ?
 C22 O5 Al1 137.04(14) . . ?
 C19 O4 Na1 111.98(12) . 2_665 ?
 C19 O4 C21 116.54(17) . . ?
 C21 O4 Na1 126.42(14) . 2_665 ?
 Na1 O6 Na1 91.26(6) . 2_665 ?
 C22 O6 Na1 143.55(14) . . ?
 C22 O6 Na1 125.18(13) . 2_665 ?
 C2 O1 Na1 110.81(12) . 2_665 ?
 C2 O1 C1 116.61(18) . . ?
 C1 O1 Na1 126.84(15) . 2_665 ?
 C14 N2 Al1 123.19(13) . . ?
 C14 N2 C13 113.99(16) . . ?
 C13 N2 Al1 122.51(13) . . ?
 C8 N1 Al1 122.42(15) . . ?
 C8 N1 C9 114.74(17) . . ?
 C9 N1 Al1 122.73(13) . . ?
 O3 C20 C15 123.55(18) . . ?
 O3 C20 C19 118.84(17) . . ?
 C15 C20 C19 117.58(17) . . ?
 N2 C14 C15 126.49(17) . . ?
 O2 C7 C6 123.57(18) . . ?
 O2 C7 C2 118.86(19) . . ?
 C6 C7 C2 117.54(18) . . ?
 C20 C15 C14 121.72(17) . . ?
 C20 C15 C16 120.25(18) . . ?
 C16 C15 C14 117.64(18) . . ?
 O7 C24 C25 118.44(18) . . ?
 O8 C24 O7 122.52(19) . . ?
 O8 C24 C25 119.04(19) . . ?
 O5 C22 C23 113.44(18) . . ?
 O6 C22 O5 125.85(19) . . ?
 O6 C22 C23 120.71(18) . . ?
 O4 C19 C20 113.64(17) . . ?
 O4 C19 C18 124.96(19) . . ?
 C18 C19 C20 121.40(18) . . ?
 C9 C10 C13 110.17(17) . . ?
 C9 C10 C11 112.40(18) . . ?
 C9 C10 C12 106.62(16) . . ?
 C13 C10 C11 111.18(17) . . ?
 C13 C10 C12 106.45(17) . . ?
 C11 C10 C12 109.74(17) . . ?
 C7 C6 C8 121.24(18) . . ?
 C7 C6 C5 120.6(2) . . ?
 C5 C6 C8 117.8(2) . . ?
 N1 C8 C6 127.6(2) . . ?
 O1 C2 C7 113.67(18) . . ?
 O1 C2 C3 125.3(2) . . ?
 C3 C2 C7 121.0(2) . . ?
 C16 C17 C18 120.2(2) . . ?
 N1 C9 C10 115.31(16) . . ?
 N2 C13 C10 114.83(16) . . ?
 C17 C16 C15 120.6(2) . . ?
 C19 C18 C17 120.0(2) . . ?
 C2 C3 C4 120.5(2) . . ?
 C5 C4 C3 120.1(2) . . ?
 C4 C5 C6 120.2(2) . . ?
 Cl5S C2S Cl4S 111.64(14) . . ?
 Cl1S C1S Cl3S 103.5(2) . . ?
 Cl2S C1S Cl1S 121.3(2) . . ?


_ins_header
;
TITL 013RWFK20 in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  10.796037  11.940873  14.619565  66.0335  84.0984  69.3612
ZERR    3.00   0.000511   0.000807   0.000691   0.0054   0.0039   0.0052
LATT  1
SFAC C H N O Na Al
UNIT 75.00 99.00 6.00 24.00 3.00 3.00
TREF
HKLF 4
END
;
_olex2_submission_original_sample_id  013RWFK20
_olex2_submission_special_instructions  'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max  1.220
_oxdiff_exptl_absorpt_empirical_full_min  0.856

data_063ap20
_audit_creation_date               2021-07-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      '12 Mansfield Road, OX1 3TA'
_audit_contact_author_email        'Charlotte.Williams@chem.ox.ac.uk'
_audit_contact_author_name         'Charlotte Williams'
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           'C50 H60 Al2 K2 N4 O16, C H Cl3'
_chemical_formula_sum              'C51 H61 Al2 Cl3 K2 N4 O16'
_chemical_formula_weight           1224.54
_chemical_melting_point            ?
_chemical_oxdiff_formula           'C30 H40 O8 N2 Co1 K1'
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        triclinic
_space_group_IT_number             2
_space_group_name_H-M_alt          'P -1'
_space_group_name_Hall             '-P 1'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                     12.4551(6)
_cell_length_b                     15.8089(10)
_cell_length_c                     16.1748(8)
_cell_angle_alpha                  65.273(5)
_cell_angle_beta                   82.478(4)
_cell_angle_gamma                  76.607(5)
_cell_volume                       2812.1(3)
_cell_formula_units_Z              2
_cell_measurement_reflns_used      5456
_cell_measurement_temperature      150.01(10)
_cell_measurement_theta_max        27.6510
_cell_measurement_theta_min        1.9880
_shelx_estimated_absorpt_T_max     0.970
_shelx_estimated_absorpt_T_min     0.935
_exptl_absorpt_coefficient_mu      0.414
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.96848
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              'clear yellow'
_exptl_crystal_colour_lustre       clear
_exptl_crystal_colour_modifier     .
_exptl_crystal_colour_primary      yellow
_exptl_crystal_density_diffrn      1.446
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               1276
_exptl_crystal_preparation         ?
_exptl_crystal_recrystallization_method  ?
_exptl_crystal_size_max            0.165
_exptl_crystal_size_mid            0.11
_exptl_crystal_size_min            0.075
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0401
_diffrn_reflns_av_unetI/netI       0.0953
_diffrn_reflns_Laue_measured_fraction_full  1.000
_diffrn_reflns_Laue_measured_fraction_max  0.874
_diffrn_reflns_limit_h_max         17
_diffrn_reflns_limit_h_min         -16
_diffrn_reflns_limit_k_max         21
_diffrn_reflns_limit_k_min         -21
_diffrn_reflns_limit_l_max         17
_diffrn_reflns_limit_l_min         -21
_diffrn_reflns_number              21284
_diffrn_reflns_point_group_measured_fraction_full  1.000
_diffrn_reflns_point_group_measured_fraction_max  0.874
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           29.663
_diffrn_reflns_theta_min           1.682
_diffrn_ambient_environment        N~2~
_diffrn_ambient_temperature        150.01(10)
_diffrn_detector                   'CCD plate'
_diffrn_detector_area_resol_mean   10.5035
_diffrn_detector_type              Atlas
_diffrn_measured_fraction_theta_full  1.000
_diffrn_measured_fraction_theta_max  0.874
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -19.00 105.00   1.00   67.50    --   21.82  77.00 150.00  124
  2  ω    -11.00 104.00   1.00   67.50    --   21.82  77.00  30.00  115
  3  ω    -14.00 105.00   1.00   67.50    --   21.82  77.00 -90.00  119
;
_diffrn_measurement_device         'four-circle diffractometer'
_diffrn_measurement_device_type    'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_type        
 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11        0.0158839000
_diffrn_orient_matrix_UB_12        0.0390501000
_diffrn_orient_matrix_UB_13        0.0026582000
_diffrn_orient_matrix_UB_21        -0.0520469000
_diffrn_orient_matrix_UB_22        0.0287483000
_diffrn_orient_matrix_UB_23        -0.0160607000
_diffrn_orient_matrix_UB_31        -0.0216998000
_diffrn_orient_matrix_UB_32        -0.0136562000
_diffrn_orient_matrix_UB_33        0.0454895000
_diffrn_radiation_monochromator    mirror
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'micro-focus sealed X-ray tube'
_diffrn_source_type                'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  8926
_reflns_number_total               13911
_reflns_odcompleteness_completeness  99.95
_reflns_odcompleteness_iscentric   1
_reflns_odcompleteness_theta       27.42
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection         'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction          'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.376
_refine_diff_density_min           -0.388
_refine_diff_density_rms           0.074
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.046
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       715
_refine_ls_number_reflns           13911
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.1083
_refine_ls_R_factor_gt             0.0609
_refine_ls_restrained_S_all        1.046
_refine_ls_shift/su_max            0.001
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0326P)²+0.5347P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1058
_refine_ls_wR_factor_ref           0.1294
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1S(H1S)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C13(H13A,H13B), C38(H38A,H38B), C34(H34A,H34B)
2.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C33(H33), C8(H8), C5(H5), C30(H30), C16(H16), C3(H3), C28(H28),
 C39(H39), C17(H17), C18(H18), C41(H41), C29(H29), C4(H4), C43(H43), C42(H42)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C1(H1A,H1B,H1C), C37(H37A,H37B,H37C), C26(H26A,H26B,
 H26C), C48(H48A,H48B,H48C), C11(H11A,H11B,H11C), C25(H25A,H25B,H25C), C36(H36A,
 H36B,H36C), C50(H50A,H50B,H50C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C),
 C46(H46A,H46B,H46C)
;
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 K1 K 0.75087(5) 0.73941(5) 0.36560(4) 0.02793(16) Uani 1 1 d . . . . .
 K2 K 0.78075(6) 0.56222(5) 0.26385(4) 0.03046(17) Uani 1 1 d . . . . .
 Cl3S Cl 0.27478(7) 0.71094(6) 0.81665(6) 0.0374(2) Uani 1 1 d . . . . .
 Cl4S Cl 0.36642(7) 0.82200(6) 0.88214(6) 0.0418(2) Uani 1 1 d . . . . .
 Al1 Al 0.66197(7) 0.63009(6) 0.60563(6) 0.01993(19) Uani 1 1 d . . . . .
 Al2 Al 0.81874(7) 0.72698(6) 0.03955(6) 0.0222(2) Uani 1 1 d . . . . .
 Cl2S Cl 0.23948(8) 0.91507(7) 0.72003(7) 0.0551(3) Uani 1 1 d . . . . .
 O2 O 0.58979(15) 0.70965(13) 0.49995(12) 0.0217(4) Uani 1 1 d . . . . .
 O15 O 0.81047(15) 0.84595(13) 0.04623(13) 0.0229(4) Uani 1 1 d . . . . .
 O7 O 0.63663(15) 0.72153(13) 0.65448(13) 0.0228(4) Uani 1 1 d . . . . .
 O10 O 0.91362(15) 0.66195(13) 0.13522(13) 0.0222(4) Uani 1 1 d . . . . .
 O3 O 0.79447(15) 0.66077(13) 0.54690(13) 0.0226(4) Uani 1 1 d . . . . .
 O5 O 0.67851(15) 0.51983(13) 0.58109(13) 0.0236(4) Uani 1 1 d . . . . .
 O13 O 0.83507(16) 0.62208(14) 0.01000(13) 0.0267(5) Uani 1 1 d . . . . .
 O11 O 0.69462(15) 0.70261(14) 0.11426(14) 0.0264(5) Uani 1 1 d . . . . .
 O1 O 0.55811(16) 0.86674(14) 0.35117(13) 0.0279(5) Uani 1 1 d . . . . .
 O4 O 0.91830(16) 0.78185(14) 0.43846(14) 0.0294(5) Uani 1 1 d . . . . .
 O9 O 0.95568(16) 0.61746(14) 0.30585(13) 0.0293(5) Uani 1 1 d . . . . .
 O6 O 0.74044(18) 0.55531(15) 0.43624(14) 0.0361(5) Uani 1 1 d . . . . .
 O12 O 0.57764(17) 0.68379(16) 0.26687(15) 0.0358(6) Uani 1 1 d . . . . .
 O14 O 0.80431(18) 0.49494(15) 0.13530(14) 0.0349(5) Uani 1 1 d . . . . .
 O8 O 0.55720(18) 0.84775(15) 0.68209(15) 0.0378(6) Uani 1 1 d . . . . .
 O16 O 0.77882(18) 0.82782(15) 0.19171(14) 0.0363(5) Uani 1 1 d . . . . .
 N2 N 0.74312(19) 0.53993(16) 0.72141(15) 0.0211(5) Uani 1 1 d . . . . .
 N1 N 0.51173(19) 0.59930(16) 0.67023(15) 0.0218(5) Uani 1 1 d . . . . .
 N3 N 0.95546(19) 0.76086(16) -0.04552(16) 0.0247(6) Uani 1 1 d . . . . .
 N4 N 0.71992(19) 0.80177(17) -0.06921(16) 0.0256(6) Uani 1 1 d . . . . .
 C32 C 0.9924(2) 0.69680(19) 0.14891(19) 0.0210(6) Uani 1 1 d . . . . .
 C20 C 0.8782(2) 0.66833(19) 0.58334(19) 0.0210(6) Uani 1 1 d . . . . .
 C7 C 0.4927(2) 0.7664(2) 0.49336(19) 0.0224(6) Uani 1 1 d . . . . .
 C14 C 0.8386(2) 0.5470(2) 0.73629(19) 0.0240(6) Uani 1 1 d . . . . .
 H14 H 0.868494 0.504843 0.791966 0.029 Uiso 1 1 calc R . . . .
 C49 C 0.8076(2) 0.8715(2) 0.1126(2) 0.0245(6) Uani 1 1 d . . . . .
 C15 C 0.9044(2) 0.6144(2) 0.67483(19) 0.0215(6) Uani 1 1 d . . . . .
 C24 C 0.6138(2) 0.8118(2) 0.6329(2) 0.0245(6) Uani 1 1 d . . . . .
 C19 C 0.9487(2) 0.7309(2) 0.5276(2) 0.0241(6) Uani 1 1 d . . . . .
 C6 C 0.4082(2) 0.7463(2) 0.5604(2) 0.0238(6) Uani 1 1 d . . . . .
 C27 C 1.0185(2) 0.6759(2) 0.23862(19) 0.0242(6) Uani 1 1 d . . . . .
 C31 C 1.0555(2) 0.7532(2) 0.0773(2) 0.0246(6) Uani 1 1 d . . . . .
 C33 C 1.0392(2) 0.77248(19) -0.0160(2) 0.0253(7) Uani 1 1 d . . . . .
 H33 H 1.094562 0.795485 -0.058633 0.030 Uiso 1 1 calc R . . . .
 C8 C 0.4214(2) 0.6587(2) 0.6411(2) 0.0242(6) Uani 1 1 d . . . . .
 H8 H 0.357482 0.643757 0.675842 0.029 Uiso 1 1 calc R . . . .
 C45 C 0.6025(2) 0.7655(2) 0.1081(2) 0.0269(7) Uani 1 1 d . . . . .
 C2 C 0.4707(2) 0.8523(2) 0.4139(2) 0.0245(6) Uani 1 1 d . . . . .
 C9 C 0.4987(2) 0.5133(2) 0.75278(19) 0.0269(7) Uani 1 1 d . . . . .
 H9A H 0.507195 0.460396 0.735194 0.032 Uiso 1 1 calc R . . . .
 H9B H 0.424265 0.523080 0.778284 0.032 Uiso 1 1 calc R . . . .
 C47 C 0.8280(2) 0.5337(2) 0.0536(2) 0.0275(7) Uani 1 1 d . . . . .
 C5 C 0.3052(2) 0.8094(2) 0.5480(2) 0.0307(7) Uani 1 1 d . . . . .
 H5 H 0.249190 0.795012 0.592648 0.037 Uiso 1 1 calc R . . . .
 C30 C 1.1394(2) 0.7882(2) 0.0965(2) 0.0302(7) Uani 1 1 d . . . . .
 H30 H 1.182074 0.824230 0.048962 0.036 Uiso 1 1 calc R . . . .
 C16 C 0.9995(2) 0.6205(2) 0.7090(2) 0.0288(7) Uani 1 1 d . . . . .
 H16 H 1.016679 0.583178 0.769538 0.035 Uiso 1 1 calc R . . . .
 C13 C 0.6982(2) 0.4592(2) 0.7921(2) 0.0267(7) Uani 1 1 d . . . . .
 H13A H 0.746195 0.429518 0.843427 0.032 Uiso 1 1 calc R . . . .
 H13B H 0.699546 0.412541 0.767543 0.032 Uiso 1 1 calc R . . . .
 C3 C 0.3702(2) 0.9128(2) 0.4038(2) 0.0316(7) Uani 1 1 d . . . . .
 H3 H 0.357437 0.968724 0.351636 0.038 Uiso 1 1 calc R . . . .
 C28 C 1.0980(2) 0.7129(2) 0.2556(2) 0.0305(7) Uani 1 1 d . . . . .
 H28 H 1.111509 0.700043 0.315316 0.037 Uiso 1 1 calc R . . . .
 C22 C 0.7138(2) 0.4993(2) 0.5118(2) 0.0261(7) Uani 1 1 d . . . . .
 C35 C 0.8633(2) 0.8507(2) -0.1959(2) 0.0292(7) Uani 1 1 d . . . . .
 C10 C 0.5801(2) 0.4864(2) 0.8265(2) 0.0256(7) Uani 1 1 d . . . . .
 C39 C 0.6214(2) 0.8443(2) -0.0597(2) 0.0290(7) Uani 1 1 d . . . . .
 H39 H 0.583474 0.883211 -0.112602 0.035 Uiso 1 1 calc R . . . .
 C12 C 0.5695(3) 0.5653(2) 0.8606(2) 0.0300(7) Uani 1 1 d . . . . .
 H12A H 0.581877 0.622690 0.810410 0.045 Uiso 1 1 calc GR . . . .
 H12B H 0.623336 0.546469 0.905617 0.045 Uiso 1 1 calc GR . . . .
 H12C H 0.496788 0.576089 0.887101 0.045 Uiso 1 1 calc GR . . . .
 C17 C 1.0669(2) 0.6811(2) 0.6537(2) 0.0321(7) Uani 1 1 d . . . . .
 H17 H 1.129618 0.684787 0.676562 0.038 Uiso 1 1 calc R . . . .
 C18 C 1.0407(2) 0.7375(2) 0.5622(2) 0.0291(7) Uani 1 1 d . . . . .
 H18 H 1.085531 0.779476 0.524876 0.035 Uiso 1 1 calc R . . . .
 C44 C 0.5352(2) 0.7579(2) 0.1883(2) 0.0305(7) Uani 1 1 d . . . . .
 C1 C 0.5441(3) 0.9546(2) 0.2724(2) 0.0340(8) Uani 1 1 d . . . . .
 H1A H 0.610971 0.957935 0.235181 0.051 Uiso 1 1 calc GR . . . .
 H1B H 0.527301 1.006561 0.291066 0.051 Uiso 1 1 calc GR . . . .
 H1C H 0.484598 0.958167 0.238117 0.051 Uiso 1 1 calc GR . . . .
 C40 C 0.5633(2) 0.8372(2) 0.0261(2) 0.0285(7) Uani 1 1 d . . . . .
 C41 C 0.4610(2) 0.8995(2) 0.0238(2) 0.0357(8) Uani 1 1 d . . . . .
 H41 H 0.435150 0.946074 -0.031687 0.043 Uiso 1 1 calc R . . . .
 C37 C 0.8542(3) 0.9453(2) -0.1877(2) 0.0350(8) Uani 1 1 d . . . . .
 H37A H 0.792756 0.990379 -0.221323 0.053 Uiso 1 1 calc GR . . . .
 H37B H 0.920927 0.969043 -0.211770 0.053 Uiso 1 1 calc GR . . . .
 H37C H 0.843134 0.935653 -0.124729 0.053 Uiso 1 1 calc GR . . . .
 C29 C 1.1587(3) 0.7698(2) 0.1839(2) 0.0350(8) Uani 1 1 d . . . . .
 H29 H 1.212299 0.795227 0.195705 0.042 Uiso 1 1 calc R . . . .
 C38 C 0.7571(3) 0.8120(2) -0.1629(2) 0.0339(8) Uani 1 1 d . . . . .
 H38A H 0.699070 0.854197 -0.204022 0.041 Uiso 1 1 calc R . . . .
 H38B H 0.768361 0.750465 -0.165738 0.041 Uiso 1 1 calc R . . . .
 C34 C 0.9609(2) 0.7771(2) -0.14231(19) 0.0309(7) Uani 1 1 d . . . . .
 H34A H 0.963031 0.717331 -0.146631 0.037 Uiso 1 1 calc R . . . .
 H34B H 1.029000 0.798261 -0.170260 0.037 Uiso 1 1 calc R . . . .
 C4 C 0.2867(3) 0.8907(2) 0.4717(2) 0.0359(8) Uani 1 1 d . . . . .
 H4 H 0.218501 0.931907 0.464552 0.043 Uiso 1 1 calc R . . . .
 C43 C 0.4377(2) 0.8208(3) 0.1843(3) 0.0398(9) Uani 1 1 d . . . . .
 H43 H 0.396022 0.815884 0.237682 0.048 Uiso 1 1 calc R . . . .
 C42 C 0.3999(3) 0.8921(3) 0.1015(3) 0.0400(9) Uani 1 1 d . . . . .
 H42 H 0.333437 0.934325 0.099571 0.048 Uiso 1 1 calc R . . . .
 C26 C 0.9982(3) 0.5715(2) 0.39529(19) 0.0329(8) Uani 1 1 d . . . . .
 H26A H 0.995064 0.618010 0.419645 0.049 Uiso 1 1 calc GR . . . .
 H26B H 1.073398 0.539872 0.392360 0.049 Uiso 1 1 calc GR . . . .
 H26C H 0.954584 0.525871 0.433920 0.049 Uiso 1 1 calc GR . . . .
 C48 C 0.8554(3) 0.4771(2) -0.0047(2) 0.0380(8) Uani 1 1 d . . . . .
 H48A H 0.839513 0.518621 -0.066851 0.057 Uiso 1 1 calc GR . . . .
 H48B H 0.811826 0.428769 0.016512 0.057 Uiso 1 1 calc GR . . . .
 H48C H 0.932400 0.448060 -0.000609 0.057 Uiso 1 1 calc GR . . . .
 C11 C 0.5548(3) 0.3957(2) 0.9061(2) 0.0356(8) Uani 1 1 d . . . . .
 H11A H 0.479309 0.407320 0.927153 0.053 Uiso 1 1 calc GR . . . .
 H11B H 0.602716 0.378278 0.955006 0.053 Uiso 1 1 calc GR . . . .
 H11C H 0.566588 0.345111 0.885912 0.053 Uiso 1 1 calc GR . . . .
 C25 C 0.6631(3) 0.8740(2) 0.5437(2) 0.0327(7) Uani 1 1 d . . . . .
 H25A H 0.738832 0.872302 0.551324 0.049 Uiso 1 1 calc GR . . . .
 H25B H 0.622411 0.938101 0.525119 0.049 Uiso 1 1 calc GR . . . .
 H25C H 0.659355 0.851049 0.497976 0.049 Uiso 1 1 calc GR . . . .
 C1S C 0.3333(3) 0.8125(2) 0.7842(2) 0.0334(8) Uani 1 1 d . . . . .
 H1S H 0.400927 0.806194 0.746928 0.040 Uiso 1 1 calc R . . . .
 C36 C 0.8845(3) 0.8646(2) -0.2960(2) 0.0415(9) Uani 1 1 d . . . . .
 H36A H 0.826138 0.912135 -0.331766 0.062 Uiso 1 1 calc GR . . . .
 H36B H 0.886782 0.805715 -0.300916 0.062 Uiso 1 1 calc GR . . . .
 H36C H 0.953748 0.884483 -0.317825 0.062 Uiso 1 1 calc GR . . . .
 C50 C 0.8441(3) 0.9640(2) 0.0857(2) 0.0431(9) Uani 1 1 d . . . . .
 H50A H 0.920265 0.951622 0.099636 0.065 Uiso 1 1 calc GR . . . .
 H50B H 0.799739 0.998814 0.118697 0.065 Uiso 1 1 calc GR . . . .
 H50C H 0.835739 1.000635 0.021489 0.065 Uiso 1 1 calc GR . . . .
 C21 C 0.9729(3) 0.8582(2) 0.3832(2) 0.0430(9) Uani 1 1 d . . . . .
 H21A H 1.050404 0.833782 0.378037 0.064 Uiso 1 1 calc GR . . . .
 H21B H 0.962255 0.902965 0.410759 0.064 Uiso 1 1 calc GR . . . .
 H21C H 0.942702 0.889162 0.323776 0.064 Uiso 1 1 calc GR . . . .
 C23 C 0.7225(3) 0.3973(2) 0.5262(2) 0.0437(9) Uani 1 1 d . . . . .
 H23A H 0.731837 0.357007 0.589573 0.066 Uiso 1 1 calc GR . . . .
 H23B H 0.784855 0.379350 0.491150 0.066 Uiso 1 1 calc GR . . . .
 H23C H 0.656343 0.390677 0.506897 0.066 Uiso 1 1 calc GR . . . .
 C46 C 0.5009(3) 0.6579(3) 0.3433(2) 0.0437(9) Uani 1 1 d . . . . .
 H46A H 0.535020 0.601025 0.391585 0.066 Uiso 1 1 calc GR . . . .
 H46B H 0.436616 0.646999 0.325359 0.066 Uiso 1 1 calc GR . . . .
 H46C H 0.479760 0.708345 0.364035 0.066 Uiso 1 1 calc GR . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 K1 O2 2.7220(19) . ?
 K1 O3 2.738(2) . ?
 K1 O1 2.718(2) . ?
 K1 O4 2.853(2) . ?
 K1 O9 3.129(2) . ?
 K1 O6 2.673(2) . ?
 K1 O12 3.307(2) . ?
 K1 O16 2.582(2) . ?
 K2 O10 2.668(2) . ?
 K2 O11 2.649(2) . ?
 K2 O9 2.781(2) . ?
 K2 O6 2.728(2) . ?
 K2 O12 2.809(2) . ?
 K2 O14 2.662(2) . ?
 K2 C16 3.409(3) 2_766 ?
 Cl3S C1S 1.768(3) . ?
 Cl4S C1S 1.761(3) . ?
 Al1 O2 1.842(2) . ?
 Al1 O7 1.869(2) . ?
 Al1 O3 1.854(2) . ?
 Al1 O5 1.905(2) . ?
 Al1 N2 2.038(2) . ?
 Al1 N1 2.077(2) . ?
 Al2 O15 1.907(2) . ?
 Al2 O10 1.853(2) . ?
 Al2 O13 1.871(2) . ?
 Al2 O11 1.843(2) . ?
 Al2 N3 2.067(2) . ?
 Al2 N4 2.040(2) . ?
 Cl2S C1S 1.762(3) . ?
 O2 C7 1.316(3) . ?
 O15 C49 1.290(3) . ?
 O7 C24 1.288(3) . ?
 O10 C32 1.313(3) . ?
 O3 C20 1.314(3) . ?
 O5 C22 1.290(3) . ?
 O13 C47 1.293(3) . ?
 O11 C45 1.316(3) . ?
 O1 C2 1.378(3) . ?
 O1 C1 1.431(3) . ?
 O4 C19 1.379(3) . ?
 O4 C21 1.427(3) . ?
 O9 C27 1.386(3) . ?
 O9 C26 1.430(3) . ?
 O6 C22 1.230(3) . ?
 O12 C44 1.382(4) . ?
 O12 C46 1.434(3) . ?
 O14 C47 1.230(4) . ?
 O8 C24 1.224(3) . ?
 O16 C49 1.223(3) . ?
 N2 C14 1.282(4) . ?
 N2 C13 1.480(3) . ?
 N1 C8 1.284(3) . ?
 N1 C9 1.478(3) . ?
 N3 C33 1.282(4) . ?
 N3 C34 1.472(4) . ?
 N4 C39 1.279(3) . ?
 N4 C38 1.478(4) . ?
 C32 C27 1.412(4) . ?
 C32 C31 1.406(4) . ?
 C20 C15 1.402(4) . ?
 C20 C19 1.418(4) . ?
 C7 C6 1.398(4) . ?
 C7 C2 1.424(4) . ?
 C14 C15 1.449(4) . ?
 C49 C50 1.503(4) . ?
 C15 C16 1.410(4) . ?
 C24 C25 1.512(4) . ?
 C19 C18 1.382(4) . ?
 C6 C8 1.444(4) . ?
 C6 C5 1.410(4) . ?
 C27 C28 1.368(4) . ?
 C31 C33 1.440(4) . ?
 C31 C30 1.413(4) . ?
 C45 C44 1.427(4) . ?
 C45 C40 1.392(4) . ?
 C2 C3 1.370(4) . ?
 C9 C10 1.525(4) . ?
 C47 C48 1.511(4) . ?
 C5 C4 1.356(4) . ?
 C30 C29 1.361(4) . ?
 C16 C17 1.371(4) . ?
 C13 C10 1.533(4) . ?
 C3 C4 1.399(4) . ?
 C28 C29 1.392(4) . ?
 C22 C23 1.510(4) . ?
 C35 C37 1.534(4) . ?
 C35 C38 1.525(4) . ?
 C35 C34 1.536(4) . ?
 C35 C36 1.535(4) . ?
 C10 C12 1.535(4) . ?
 C10 C11 1.540(4) . ?
 C39 C40 1.451(4) . ?
 C17 C18 1.407(4) . ?
 C44 C43 1.370(4) . ?
 C40 C41 1.412(4) . ?
 C41 C42 1.357(5) . ?
 C43 C42 1.393(5) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O2 K1 O3 56.95(6) . . ?
 O2 K1 O4 103.52(6) . . ?
 O2 K1 O9 137.45(6) . . ?
 O2 K1 O12 82.10(5) . . ?
 O3 K1 O4 56.31(6) . . ?
 O3 K1 O9 96.57(6) . . ?
 O3 K1 O12 126.94(6) . . ?
 O1 K1 O2 57.79(6) . . ?
 O1 K1 O3 104.75(6) . . ?
 O1 K1 O4 111.48(6) . . ?
 O1 K1 O9 158.60(6) . . ?
 O1 K1 O12 73.35(6) . . ?
 O4 K1 O9 81.88(6) . . ?
 O4 K1 O12 173.93(6) . . ?
 O9 K1 O12 92.43(5) . . ?
 O6 K1 O2 71.81(6) . . ?
 O6 K1 O3 70.55(6) . . ?
 O6 K1 O1 117.58(7) . . ?
 O6 K1 O4 114.19(7) . . ?
 O6 K1 O9 67.76(6) . . ?
 O6 K1 O12 65.08(6) . . ?
 O16 K1 O2 141.42(7) . . ?
 O16 K1 O3 159.26(7) . . ?
 O16 K1 O1 86.83(7) . . ?
 O16 K1 O4 103.63(7) . . ?
 O16 K1 O9 73.45(6) . . ?
 O16 K1 O6 119.62(7) . . ?
 O16 K1 O12 72.52(7) . . ?
 O10 K2 O9 57.91(6) . . ?
 O10 K2 O6 126.76(7) . . ?
 O10 K2 O12 108.57(6) . . ?
 O10 K2 C16 83.00(7) . 2_766 ?
 O11 K2 O10 60.70(6) . . ?
 O11 K2 O9 107.20(6) . . ?
 O11 K2 O6 125.69(7) . . ?
 O11 K2 O12 57.68(6) . . ?
 O11 K2 O14 72.53(6) . . ?
 O11 K2 C16 130.65(7) . 2_766 ?
 O9 K2 O12 112.50(6) . . ?
 O9 K2 C16 74.44(7) . 2_766 ?
 O6 K2 O9 72.47(6) . . ?
 O6 K2 O12 72.15(7) . . ?
 O6 K2 C16 102.34(7) . 2_766 ?
 O12 K2 C16 168.35(7) . 2_766 ?
 O14 K2 O10 74.83(6) . . ?
 O14 K2 O9 120.95(7) . . ?
 O14 K2 O6 155.60(7) . . ?
 O14 K2 O12 114.80(7) . . ?
 O14 K2 C16 66.06(7) . 2_766 ?
 O2 Al1 O7 94.70(9) . . ?
 O2 Al1 O3 89.57(9) . . ?
 O2 Al1 O5 93.89(9) . . ?
 O2 Al1 N2 178.76(10) . . ?
 O2 Al1 N1 89.49(9) . . ?
 O7 Al1 O5 167.84(10) . . ?
 O7 Al1 N2 86.52(9) . . ?
 O7 Al1 N1 84.74(9) . . ?
 O3 Al1 O7 94.26(9) . . ?
 O3 Al1 O5 94.40(9) . . ?
 O3 Al1 N2 90.13(9) . . ?
 O3 Al1 N1 178.57(10) . . ?
 O5 Al1 N2 84.94(9) . . ?
 O5 Al1 N1 86.74(9) . . ?
 N2 Al1 N1 90.84(10) . . ?
 O15 Al2 N3 84.22(9) . . ?
 O15 Al2 N4 85.99(9) . . ?
 O10 Al2 O15 92.95(9) . . ?
 O10 Al2 O13 93.26(9) . . ?
 O10 Al2 N3 87.84(9) . . ?
 O10 Al2 N4 177.36(10) . . ?
 O13 Al2 O15 169.18(10) . . ?
 O13 Al2 N3 87.17(10) . . ?
 O13 Al2 N4 87.41(10) . . ?
 O11 Al2 O15 93.33(9) . . ?
 O11 Al2 O10 93.25(9) . . ?
 O11 Al2 O13 95.15(10) . . ?
 O11 Al2 N3 177.38(10) . . ?
 O11 Al2 N4 89.24(10) . . ?
 N4 Al2 N3 89.64(10) . . ?
 Al1 O2 K1 105.22(8) . . ?
 C7 O2 K1 124.11(17) . . ?
 C7 O2 Al1 126.60(17) . . ?
 C49 O15 Al2 133.77(19) . . ?
 C24 O7 Al1 143.00(19) . . ?
 Al2 O10 K2 100.71(8) . . ?
 C32 O10 K2 125.78(17) . . ?
 C32 O10 Al2 123.62(18) . . ?
 Al1 O3 K1 104.28(8) . . ?
 C20 O3 K1 126.57(17) . . ?
 C20 O3 Al1 126.58(17) . . ?
 C22 O5 Al1 134.60(19) . . ?
 C47 O13 Al2 136.11(19) . . ?
 Al2 O11 K2 101.68(8) . . ?
 C45 O11 K2 127.47(18) . . ?
 C45 O11 Al2 124.48(19) . . ?
 C2 O1 K1 124.60(17) . . ?
 C2 O1 C1 116.9(2) . . ?
 C1 O1 K1 118.50(17) . . ?
 C19 O4 K1 121.90(17) . . ?
 C19 O4 C21 117.6(2) . . ?
 C21 O4 K1 120.54(18) . . ?
 K2 O9 K1 77.99(5) . . ?
 C27 O9 K1 110.28(16) . . ?
 C27 O9 K2 121.67(17) . . ?
 C27 O9 C26 116.6(2) . . ?
 C26 O9 K1 92.94(15) . . ?
 C26 O9 K2 120.60(17) . . ?
 K1 O6 K2 87.32(6) . . ?
 C22 O6 K1 134.01(19) . . ?
 C22 O6 K2 138.00(19) . . ?
 K2 O12 K1 74.65(5) . . ?
 C44 O12 K1 113.44(17) . . ?
 C44 O12 K2 121.45(17) . . ?
 C44 O12 C46 115.6(2) . . ?
 C46 O12 K1 96.26(17) . . ?
 C46 O12 K2 121.0(2) . . ?
 C47 O14 K2 129.3(2) . . ?
 C49 O16 K1 169.8(2) . . ?
 C14 N2 Al1 122.2(2) . . ?
 C14 N2 C13 115.4(2) . . ?
 C13 N2 Al1 122.32(19) . . ?
 C8 N1 Al1 120.23(19) . . ?
 C8 N1 C9 114.9(2) . . ?
 C9 N1 Al1 124.80(18) . . ?
 C33 N3 Al2 120.4(2) . . ?
 C33 N3 C34 116.6(2) . . ?
 C34 N3 Al2 123.0(2) . . ?
 C39 N4 Al2 121.1(2) . . ?
 C39 N4 C38 116.0(3) . . ?
 C38 N4 Al2 122.90(18) . . ?
 O10 C32 C27 119.9(3) . . ?
 O10 C32 C31 122.7(3) . . ?
 C31 C32 C27 117.3(3) . . ?
 O3 C20 C15 123.1(3) . . ?
 O3 C20 C19 119.2(3) . . ?
 C15 C20 C19 117.7(3) . . ?
 O2 C7 C6 123.2(3) . . ?
 O2 C7 C2 119.1(3) . . ?
 C6 C7 C2 117.7(3) . . ?
 N2 C14 C15 126.4(3) . . ?
 O15 C49 C50 113.9(3) . . ?
 O16 C49 O15 126.1(3) . . ?
 O16 C49 C50 120.0(3) . . ?
 C20 C15 C14 121.5(3) . . ?
 C20 C15 C16 120.8(3) . . ?
 C16 C15 C14 117.6(3) . . ?
 O7 C24 C25 117.2(3) . . ?
 O8 C24 O7 122.9(3) . . ?
 O8 C24 C25 119.8(3) . . ?
 O4 C19 C20 114.8(2) . . ?
 O4 C19 C18 124.2(3) . . ?
 C18 C19 C20 121.0(3) . . ?
 C7 C6 C8 121.4(3) . . ?
 C7 C6 C5 120.1(3) . . ?
 C5 C6 C8 118.4(3) . . ?
 O9 C27 C32 114.3(3) . . ?
 C28 C27 O9 124.1(3) . . ?
 C28 C27 C32 121.6(3) . . ?
 C32 C31 C33 120.9(3) . . ?
 C32 C31 C30 119.9(3) . . ?
 C30 C31 C33 119.1(3) . . ?
 N3 C33 C31 125.9(3) . . ?
 N1 C8 C6 127.2(3) . . ?
 O11 C45 C44 119.1(3) . . ?
 O11 C45 C40 123.6(3) . . ?
 C40 C45 C44 117.3(3) . . ?
 O1 C2 C7 114.0(2) . . ?
 C3 C2 O1 125.0(3) . . ?
 C3 C2 C7 121.0(3) . . ?
 N1 C9 C10 114.6(2) . . ?
 O13 C47 C48 113.9(3) . . ?
 O14 C47 O13 125.6(3) . . ?
 O14 C47 C48 120.4(3) . . ?
 C4 C5 C6 120.9(3) . . ?
 C29 C30 C31 120.8(3) . . ?
 C15 C16 K2 115.78(18) . 2_766 ?
 C17 C16 K2 87.93(18) . 2_766 ?
 C17 C16 C15 120.5(3) . . ?
 N2 C13 C10 114.4(2) . . ?
 C2 C3 C4 120.2(3) . . ?
 C27 C28 C29 120.3(3) . . ?
 O5 C22 C23 116.2(3) . . ?
 O6 C22 O5 125.7(3) . . ?
 O6 C22 C23 118.1(3) . . ?
 C37 C35 C34 110.5(3) . . ?
 C37 C35 C36 110.0(3) . . ?
 C38 C35 C37 111.7(2) . . ?
 C38 C35 C34 109.9(2) . . ?
 C38 C35 C36 107.1(3) . . ?
 C36 C35 C34 107.5(2) . . ?
 C9 C10 C13 110.1(2) . . ?
 C9 C10 C12 112.0(2) . . ?
 C9 C10 C11 107.3(2) . . ?
 C13 C10 C12 111.8(2) . . ?
 C13 C10 C11 105.9(2) . . ?
 C12 C10 C11 109.5(2) . . ?
 N4 C39 C40 126.0(3) . . ?
 C16 C17 C18 119.6(3) . . ?
 C19 C18 C17 120.3(3) . . ?
 O12 C44 C45 114.3(3) . . ?
 C43 C44 O12 125.0(3) . . ?
 C43 C44 C45 120.8(3) . . ?
 C45 C40 C39 120.8(3) . . ?
 C45 C40 C41 120.6(3) . . ?
 C41 C40 C39 118.4(3) . . ?
 C42 C41 C40 120.9(3) . . ?
 C30 C29 C28 119.9(3) . . ?
 N4 C38 C35 114.0(2) . . ?
 N3 C34 C35 113.6(2) . . ?
 C5 C4 C3 120.0(3) . . ?
 C44 C43 C42 121.0(3) . . ?
 C41 C42 C43 119.4(3) . . ?
 Cl4S C1S Cl3S 109.55(17) . . ?
 Cl4S C1S Cl2S 109.94(18) . . ?
 Cl2S C1S Cl3S 109.96(17) . . ?

_olex2_submission_special_instructions  'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max  1.236
_oxdiff_exptl_absorpt_empirical_full_min  0.897

data_014rwfk20
_audit_creation_date               2021-03-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      '12 Mansfield Road, OX1 3TA'
_audit_contact_author_email        'Charlotte.Williams@chem.ox.ac.uk'
_audit_contact_author_name         'Charlotte Williams'
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           'C50 H60 Al2 N4 O16 Rb2, C H Cl3'
_chemical_formula_sum              'C51 H61 Al2 Cl3 N4 O16 Rb2'
_chemical_formula_weight           1317.28
_chemical_melting_point            ?
_chemical_oxdiff_formula           C100H100Al1N2O8Rb1
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Al' 'Al' 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Rb' 'Rb' -0.4688 1.6079
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        triclinic
_space_group_IT_number             2
_space_group_name_H-M_alt          'P -1'
_space_group_name_Hall             '-P 1'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                     12.5460(3)
_cell_length_b                     15.7343(4)
_cell_length_c                     16.4513(5)
_cell_angle_alpha                  64.372(3)
_cell_angle_beta                   82.396(2)
_cell_angle_gamma                  76.638(2)
_cell_volume                       2846.84(15)
_cell_formula_units_Z              2
_cell_measurement_reflns_used      18002
_cell_measurement_temperature      149.99(10)
_cell_measurement_theta_max        76.5160
_cell_measurement_theta_min        2.9770
_shelx_estimated_absorpt_T_max     0.612
_shelx_estimated_absorpt_T_min     0.303
_exptl_absorpt_coefficient_mu      4.422
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.73130
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              'clear light yellow'
_exptl_crystal_colour_lustre       clear
_exptl_crystal_colour_modifier     light
_exptl_crystal_colour_primary      yellow
_exptl_crystal_density_diffrn      1.537
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               1348
_exptl_crystal_preparation         ?
_exptl_crystal_size_max            0.355
_exptl_crystal_size_mid            0.203
_exptl_crystal_size_min            0.123
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0319
_diffrn_reflns_av_unetI/netI       0.0357
_diffrn_reflns_Laue_measured_fraction_full  1.000
_diffrn_reflns_Laue_measured_fraction_max  0.987
_diffrn_reflns_limit_h_max         15
_diffrn_reflns_limit_h_min         -13
_diffrn_reflns_limit_k_max         19
_diffrn_reflns_limit_k_min         -19
_diffrn_reflns_limit_l_max         18
_diffrn_reflns_limit_l_min         -20
_diffrn_reflns_number              30073
_diffrn_reflns_point_group_measured_fraction_full  1.000
_diffrn_reflns_point_group_measured_fraction_max  0.987
_diffrn_reflns_theta_full          67.684
_diffrn_reflns_theta_max           76.599
_diffrn_reflns_theta_min           2.981
_diffrn_ambient_environment        N~2~
_diffrn_ambient_temperature        149.99(10)
_diffrn_detector                   'CCD plate'
_diffrn_detector_area_resol_mean   10.5035
_diffrn_detector_type              Atlas
_diffrn_measured_fraction_theta_full  1.000
_diffrn_measured_fraction_theta_max  0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω     43.00  94.00   1.00    1.00    --    0.00  19.00  90.00   51
  2  ω    -15.00  39.00   1.00    1.00    --    0.00 -77.00 -90.00   54
  3  ω     -7.00  35.00   1.00    1.00    --    0.00 -77.00 120.00   42
  4  ω     -3.00  30.00   1.00    1.00    --    0.00  19.00  90.00   33
  5  ω   -153.00  29.00   1.00    2.00    --  -60.50 -15.00  60.00  182
  6  ω    -87.00 -32.00   1.00    2.00    --  -60.50 125.00  60.00   55
  7  ω      1.00  31.00   1.00    2.00    --  -60.50  30.00 -60.00   30
  8  ω     97.00 143.00   1.00    2.00    --   60.50 125.00  30.00   46
  9  ω     97.00 148.00   1.00    2.00    --   60.50 125.00 150.00   51
 10  ω    107.00 155.00   1.00    2.00    --   60.50  77.00 120.00   48
 11  ω    103.00 133.00   1.00    2.00    --   60.50 125.00-180.00   30
 12  ω    114.00 150.00   1.00    2.00    --   60.50 125.00 -60.00   36
 13  ω     29.00 111.00   1.00    2.00    --   60.50-125.00   0.00   82
 14  ω     99.00 151.00   1.00    2.00    --   60.50 135.00 -20.00   52
 15  ω    101.00 126.00   1.00    2.00    --   60.50 125.00 -90.00   25
 16  ω     47.00  89.00   1.00    3.00    --  121.00 -91.00-150.00   42
 17  ω     60.00 108.00   1.00    3.00    --  121.00-111.00  30.00   48
 18  ω     31.00  64.00   1.00    3.00    --  121.00 -37.00 120.00   33
 19  ω     32.00 106.00   1.00    3.00    --  121.00-111.00  90.00   74
 20  ω     68.00 108.00   1.00    3.00    --  121.00-111.00  60.00   40
 21  ω     48.00  85.00   1.00    3.00    --  121.00 -63.00 -90.00   37
 22  ω     28.00  60.00   1.00    3.00    --  121.00 -77.00  30.00   32
 23  ω     78.00 171.00   1.00    3.00    --  121.00  63.00 120.00   93
 24  ω     30.00  57.00   1.00    3.00    --  121.00 -37.00-150.00   27
 25  ω     74.00 108.00   1.00    3.00    --  121.00-111.00-150.00   34
 26  ω     39.00 108.00   1.00    3.00    --  121.00-111.00 -60.00   69
 27  ω     29.00  59.00   1.00    3.00    --  121.00-111.00 -30.00   30
 28  ω     83.00 108.00   1.00    3.00    --  121.00-111.00 -30.00   25
 29  ω     34.00  60.00   1.00    3.00    --  121.00 -50.00  60.00   26
 30  ω    116.00 166.00   1.00    3.00    --  121.00  77.00-150.00   50
 31  ω    128.00 154.00   1.00    3.00    --  121.00  37.00 120.00   26
 32  ω    106.00 137.00   1.00    3.00    --  121.00  77.00  90.00   31
 33  ω    119.00 153.00   1.00    3.00    --  121.00 111.00 150.00   34
 34  ω     31.00  64.00   1.00    3.00    --  121.00 -37.00-180.00   33
 35  ω     55.00 107.00   1.00    3.00    --  121.00-111.00-180.00   52
 36  ω     72.00 107.00   1.00    3.00    --  121.00-111.00 150.00   35
 37  ω    151.00 177.00   1.00    3.00    --  121.00 111.00 -60.00   26
 38  ω    144.00 169.00   1.00    3.00    --  121.00  77.00  90.00   25
 39  ω    104.00 169.00   1.00    3.00    --  121.00  77.00 -30.00   65
 40  ω    110.00 136.00   1.00    3.00    --  121.00 111.00 -60.00   26
 41  ω     39.00  64.00   1.00    3.00    --  121.00 -77.00-120.00   25
 42  ω    100.00 125.00   1.00    3.00    --  121.00 -77.00-120.00   25
 43  ω     39.00  72.00   1.00    3.00    --  121.00 -50.00 -60.00   33
 44  ω     43.00  69.00   1.00    3.00    --  121.00 -50.00  90.00   26
 45  ω    103.00 165.00   1.00    3.00    --  121.00  77.00  60.00   62
 46  ω     65.00 104.00   1.00    3.00    --  121.00-111.00 -90.00   39
 47  ω     95.00 153.00   1.00    3.00    --  121.00  37.00  30.00   58
 48  ω     89.00 119.00   1.00    3.00    --  121.00 -77.00  30.00   30
 49  ω    -21.00  19.00   1.00    1.00    --    0.00  37.00 -30.00   40
 50  ω    -41.00  -1.00   1.00    1.00    --    0.00  77.00  60.00   40
 51  ω     13.00  40.00   1.00    1.00    --    0.00 -99.00-180.00   27
 52  ω      0.00  35.00   1.00    1.00    --    0.00  77.00  60.00   35
 53  ω     28.00  81.00   1.00    1.00    --    0.00  37.00 -30.00   53
 54  ω    -19.00   7.00   1.00    2.00    --   38.00 110.00 100.29   26
 55  ω     -7.00  18.00   1.00    2.00    --   42.00  94.00 155.17   25
 56  ω      4.00  29.00   1.00    2.00    --   50.00  88.00-121.46   25
 57  ω      4.00  30.00   1.00    2.00    --   50.00  89.00 -39.75   26
 58  ω     16.00  42.00   1.00    2.00    --   60.50  81.00  93.70   26
 59  ω     16.00  42.00   1.00    2.00    --   60.50  82.00  22.66   26
 60  ω     16.00  41.00   1.00    2.00    --   60.50  82.00  -6.34   25
 61  ω     16.00  41.00   1.00    2.00    --   60.50  82.00-150.75   25
 62  ω     16.00  41.00   1.00    2.00    --   60.50  82.00 152.89   25
 63  ω     16.00  41.00   1.00    2.00    --   60.50  81.00 -81.61   25
 64  ω     24.00  51.00   1.00    2.00    --   66.00  74.00  71.26   27
 65  ω     23.00 150.00   1.00    2.00    --   66.00  71.00-108.55  127
;
_diffrn_measurement_device         'four-circle diffractometer'
_diffrn_measurement_device_type    'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_type        
 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11        0.0223989000
_diffrn_orient_matrix_UB_12        0.1011763000
_diffrn_orient_matrix_UB_13        -0.0613118000
_diffrn_orient_matrix_UB_21        0.0116239000
_diffrn_orient_matrix_UB_22        0.0164235000
_diffrn_orient_matrix_UB_23        0.0839183000
_diffrn_orient_matrix_UB_31        0.1237489000
_diffrn_orient_matrix_UB_32        -0.0418377000
_diffrn_orient_matrix_UB_33        -0.0006980000
_diffrn_radiation_monochromator    mirror
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             CuK\a
_diffrn_radiation_wavelength       1.54184
_diffrn_source                     'micro-focus sealed X-ray tube'
_diffrn_source_type                'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  10423
_reflns_number_total               11825
_reflns_odcompleteness_completeness  99.79
_reflns_odcompleteness_iscentric   1
_reflns_odcompleteness_theta       74.33
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_collection         'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_reduction          'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.667
_refine_diff_density_min           -0.499
_refine_diff_density_rms           0.067
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.029
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       715
_refine_ls_number_reflns           11825
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0379
_refine_ls_R_factor_gt             0.0323
_refine_ls_restrained_S_all        1.029
_refine_ls_shift/su_max            0.002
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0477P)²+0.6245P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0844
_refine_ls_wR_factor_ref           0.0884
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1S(H1S)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C13(H13A,H13B), C38(H38A,H38B), C34(H34A,H34B)
2.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C39(H39), C8(H8), C41(H41), C33(H33), C16(H16), C5(H5), C3(H3),
 C18(H18), C30(H30), C4(H4), C43(H43), C17(H17), C42(H42), C29(H29), C28(H28)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C25(H25A,H25B,H25C), C48(H48A,H48B,H48C), C11(H11A,H11B,
 H11C), C36(H36A,H36B,H36C), C21(H21A,H21B,H21C), C46(H46A,H46B,H46C), C1(H1A,
 H1B,H1C), C23(H23A,H23B,H23C), C37(H37A,H37B,H37C), C26(H26A,H26B,H26C),
 C50(H50A,H50B,H50C)
;
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Rb2 Rb 0.22108(2) 0.45333(2) 0.72790(2) 0.02908(6) Uani 1 1 d . . . . .
 Rb1 Rb 0.24536(2) 0.25931(2) 0.63654(2) 0.02851(6) Uani 1 1 d . . . . .
 Cl2S Cl 0.72643(4) 0.28571(5) 0.18432(4) 0.03781(13) Uani 1 1 d . . . . .
 Cl4S Cl 0.63645(5) 0.17264(5) 0.12180(4) 0.04295(14) Uani 1 1 d . . . . .
 Al1 Al 0.33867(4) 0.37347(4) 0.38878(4) 0.01973(12) Uani 1 1 d . . . . .
 Al2 Al 0.18467(5) 0.27436(5) 0.95978(4) 0.02307(12) Uani 1 1 d . . . . .
 Cl3S Cl 0.76117(7) 0.07921(6) 0.28319(6) 0.0618(2) Uani 1 1 d . . . . .
 O3 O 0.41162(11) 0.29417(10) 0.49382(9) 0.0229(3) Uani 1 1 d . . . . .
 O11 O 0.08958(11) 0.33927(11) 0.86509(9) 0.0245(3) Uani 1 1 d . . . . .
 O2 O 0.20624(11) 0.34135(11) 0.44642(9) 0.0236(3) Uani 1 1 d . . . . .
 O15 O 0.19171(11) 0.15370(11) 0.95792(9) 0.0246(3) Uani 1 1 d . . . . .
 O5 O 0.31950(11) 0.48669(11) 0.40938(9) 0.0242(3) Uani 1 1 d . . . . .
 O7 O 0.36586(11) 0.28037(10) 0.34291(9) 0.0237(3) Uani 1 1 d . . . . .
 O1 O 0.07951(12) 0.22027(12) 0.55508(10) 0.0310(3) Uani 1 1 d . . . . .
 O13 O 0.16794(12) 0.38036(11) 0.98750(10) 0.0282(3) Uani 1 1 d . . . . .
 O10 O 0.30691(11) 0.29926(11) 0.88457(10) 0.0272(3) Uani 1 1 d . . . . .
 O4 O 0.44754(12) 0.13520(11) 0.64384(10) 0.0291(3) Uani 1 1 d . . . . .
 O12 O 0.04357(12) 0.38341(12) 0.69719(10) 0.0292(3) Uani 1 1 d . . . . .
 O6 O 0.25682(15) 0.45343(13) 0.55137(11) 0.0395(4) Uani 1 1 d . . . . .
 O9 O 0.42027(12) 0.31676(14) 0.73256(11) 0.0353(4) Uani 1 1 d . . . . .
 O14 O 0.19722(15) 0.51303(13) 0.86632(11) 0.0388(4) Uani 1 1 d . . . . .
 O8 O 0.44327(15) 0.15244(13) 0.31831(12) 0.0407(4) Uani 1 1 d . . . . .
 O16 O 0.22865(16) 0.16410(14) 0.81757(11) 0.0422(4) Uani 1 1 d . . . . .
 N1 N 0.25865(13) 0.46347(12) 0.27251(11) 0.0221(3) Uani 1 1 d . . . . .
 N4 N 0.04932(14) 0.24046(13) 1.04566(11) 0.0265(4) Uani 1 1 d . . . . .
 N2 N 0.48787(13) 0.40680(13) 0.32344(11) 0.0220(3) Uani 1 1 d . . . . .
 N3 N 0.28398(14) 0.19912(14) 1.06749(12) 0.0285(4) Uani 1 1 d . . . . .
 C45 C 0.01080(15) 0.30380(15) 0.85351(14) 0.0243(4) Uani 1 1 d . . . . .
 C20 C 0.50864(15) 0.23748(15) 0.50120(13) 0.0226(4) Uani 1 1 d . . . . .
 C9 C 0.30240(17) 0.54505(15) 0.20171(14) 0.0260(4) Uani 1 1 d . . . . .
 H9A H 0.300678 0.593386 0.225523 0.031 Uiso 1 1 calc R . . . .
 H9B H 0.253417 0.575385 0.150026 0.031 Uiso 1 1 calc R . . . .
 C7 C 0.12414(15) 0.33304(15) 0.41065(14) 0.0223(4) Uani 1 1 d . . . . .
 C15 C 0.59225(16) 0.25882(16) 0.43374(14) 0.0249(4) Uani 1 1 d . . . . .
 C44 C -0.01651(16) 0.32419(16) 0.76573(15) 0.0269(4) Uani 1 1 d . . . . .
 C2 C 0.05197(16) 0.26971(16) 0.46575(14) 0.0256(4) Uani 1 1 d . . . . .
 C24 C 0.38766(16) 0.18894(16) 0.36656(14) 0.0256(4) Uani 1 1 d . . . . .
 C19 C 0.53213(16) 0.15125(16) 0.58098(14) 0.0260(4) Uani 1 1 d . . . . .
 C14 C 0.57804(16) 0.34704(16) 0.35253(14) 0.0249(4) Uani 1 1 d . . . . .
 H14 H 0.642458 0.362658 0.316618 0.030 Uiso 1 1 calc R . . . .
 C40 C -0.05159(16) 0.24687(15) 0.92648(15) 0.0275(4) Uani 1 1 d . . . . .
 C39 C -0.03439(17) 0.22839(16) 1.01835(15) 0.0294(5) Uani 1 1 d . . . . .
 H39 H -0.090282 0.205232 1.062246 0.035 Uiso 1 1 calc R . . . .
 C6 C 0.09976(16) 0.38608(15) 0.31863(14) 0.0240(4) Uani 1 1 d . . . . .
 C47 C 0.17344(17) 0.46998(16) 0.94644(15) 0.0273(4) Uani 1 1 d . . . . .
 C8 C 0.16454(16) 0.45509(15) 0.25766(13) 0.0238(4) Uani 1 1 d . . . . .
 H8 H 0.134361 0.498538 0.200981 0.029 Uiso 1 1 calc R . . . .
 C10 C 0.41963(17) 0.51888(15) 0.16734(13) 0.0248(4) Uani 1 1 d . . . . .
 C12 C 0.43248(18) 0.43735(16) 0.13695(14) 0.0289(4) Uani 1 1 d . . . . .
 H12A H 0.417594 0.379042 0.188527 0.043 Uiso 1 1 calc GR . . . .
 H12B H 0.507463 0.424879 0.113159 0.043 Uiso 1 1 calc GR . . . .
 H12C H 0.380567 0.456117 0.089769 0.043 Uiso 1 1 calc GR . . . .
 C32 C 0.39840(16) 0.23610(17) 0.89056(15) 0.0276(4) Uani 1 1 d . . . . .
 C31 C 0.43833(16) 0.16385(17) 0.97286(17) 0.0308(5) Uani 1 1 d . . . . .
 C49 C 0.19494(16) 0.12439(16) 0.89559(14) 0.0262(4) Uani 1 1 d . . . . .
 C41 C -0.13565(17) 0.21063(16) 0.91054(17) 0.0344(5) Uani 1 1 d . . . . .
 H41 H -0.178687 0.174345 0.959918 0.041 Uiso 1 1 calc R . . . .
 C33 C 0.38204(17) 0.15666(17) 1.05714(16) 0.0313(5) Uani 1 1 d . . . . .
 H33 H 0.421367 0.116485 1.110430 0.038 Uiso 1 1 calc R . . . .
 C16 C 0.69534(17) 0.19596(17) 0.44571(16) 0.0315(5) Uani 1 1 d . . . . .
 H16 H 0.751428 0.211568 0.399920 0.038 Uiso 1 1 calc R . . . .
 C5 C 0.00679(17) 0.37918(17) 0.28444(15) 0.0290(4) Uani 1 1 d . . . . .
 H5 H -0.009669 0.417537 0.222846 0.035 Uiso 1 1 calc R . . . .
 C22 C 0.28228(16) 0.50910(17) 0.47535(15) 0.0271(4) Uani 1 1 d . . . . .
 C3 C -0.03738(17) 0.26249(17) 0.43055(16) 0.0307(5) Uani 1 1 d . . . . .
 H3 H -0.083783 0.219773 0.468546 0.037 Uiso 1 1 calc R . . . .
 C18 C 0.63318(18) 0.09027(18) 0.59069(16) 0.0334(5) Uani 1 1 d . . . . .
 H18 H 0.646956 0.032613 0.644057 0.040 Uiso 1 1 calc R . . . .
 C25 C 0.3385(2) 0.12606(17) 0.45549(15) 0.0326(5) Uani 1 1 d . . . . .
 H25A H 0.343564 0.149156 0.501177 0.049 Uiso 1 1 calc GR . . . .
 H25B H 0.378837 0.059618 0.474728 0.049 Uiso 1 1 calc GR . . . .
 H25C H 0.261435 0.128677 0.448149 0.049 Uiso 1 1 calc GR . . . .
 C13 C 0.50014(17) 0.49302(16) 0.24054(14) 0.0270(4) Uani 1 1 d . . . . .
 H13A H 0.575728 0.483198 0.215222 0.032 Uiso 1 1 calc R . . . .
 H13B H 0.490797 0.548203 0.256580 0.032 Uiso 1 1 calc R . . . .
 C30 C 0.54050(18) 0.10105(19) 0.97556(19) 0.0372(5) Uani 1 1 d . . . . .
 H30 H 0.567182 0.052863 1.031878 0.045 Uiso 1 1 calc R . . . .
 C4 C -0.06074(17) 0.31741(18) 0.33928(17) 0.0324(5) Uani 1 1 d . . . . .
 H4 H -0.122617 0.312070 0.315458 0.039 Uiso 1 1 calc R . . . .
 C27 C 0.46342(17) 0.24373(19) 0.81100(17) 0.0322(5) Uani 1 1 d . . . . .
 C48 C 0.1461(2) 0.52298(19) 1.00667(17) 0.0382(5) Uani 1 1 d . . . . .
 H48A H 0.067064 0.548291 1.006864 0.057 Uiso 1 1 calc GR . . . .
 H48B H 0.185689 0.576240 0.983946 0.057 Uiso 1 1 calc GR . . . .
 H48C H 0.167961 0.478748 1.068221 0.057 Uiso 1 1 calc GR . . . .
 C43 C -0.09634(18) 0.28471(18) 0.75179(17) 0.0344(5) Uani 1 1 d . . . . .
 H43 H -0.110838 0.296811 0.692127 0.041 Uiso 1 1 calc R . . . .
 C35 C 0.14293(19) 0.15001(18) 1.19365(15) 0.0341(5) Uani 1 1 d . . . . .
 C11 C 0.4442(2) 0.61009(18) 0.08737(15) 0.0349(5) Uani 1 1 d . . . . .
 H11A H 0.398095 0.625771 0.037244 0.052 Uiso 1 1 calc GR . . . .
 H11B H 0.521631 0.599313 0.068144 0.052 Uiso 1 1 calc GR . . . .
 H11C H 0.428746 0.663483 0.105587 0.052 Uiso 1 1 calc GR . . . .
 C36 C 0.1510(2) 0.05440(18) 1.18777(16) 0.0385(6) Uani 1 1 d . . . . .
 H36A H 0.083205 0.030166 1.212754 0.058 Uiso 1 1 calc GR . . . .
 H36B H 0.213156 0.007764 1.222271 0.058 Uiso 1 1 calc GR . . . .
 H36C H 0.161950 0.063958 1.124529 0.058 Uiso 1 1 calc GR . . . .
 C21 C 0.4635(2) 0.04684(17) 0.72331(16) 0.0345(5) Uani 1 1 d . . . . .
 H21A H 0.524665 0.044249 0.756212 0.052 Uiso 1 1 calc GR . . . .
 H21B H 0.480050 -0.007345 0.706148 0.052 Uiso 1 1 calc GR . . . .
 H21C H 0.396629 0.043127 0.761952 0.052 Uiso 1 1 calc GR . . . .
 C17 C 0.71533(18) 0.11254(19) 0.52282(18) 0.0376(5) Uani 1 1 d . . . . .
 H17 H 0.784518 0.070245 0.530001 0.045 Uiso 1 1 calc R . . . .
 C42 C -0.15594(19) 0.22710(19) 0.82485(19) 0.0393(6) Uani 1 1 d . . . . .
 H42 H -0.210149 0.199612 0.814943 0.047 Uiso 1 1 calc R . . . .
 C46 C -0.00057(19) 0.42860(19) 0.60880(15) 0.0342(5) Uani 1 1 d . . . . .
 H46A H -0.076573 0.461382 0.611882 0.051 Uiso 1 1 calc GR . . . .
 H46B H 0.001520 0.379730 0.586420 0.051 Uiso 1 1 calc GR . . . .
 H46C H 0.043231 0.475501 0.567794 0.051 Uiso 1 1 calc GR . . . .
 C29 C 0.60054(18) 0.1091(2) 0.8985(2) 0.0433(6) Uani 1 1 d . . . . .
 H29 H 0.668331 0.066074 0.900990 0.052 Uiso 1 1 calc R . . . .
 C28 C 0.56266(18) 0.1806(2) 0.81554(19) 0.0405(6) Uani 1 1 d . . . . .
 H28 H 0.605084 0.186205 0.761802 0.049 Uiso 1 1 calc R . . . .
 C1 C 0.0215(2) 0.1454(2) 0.61077(18) 0.0435(6) Uani 1 1 d . . . . .
 H1A H 0.049296 0.114629 0.671893 0.065 Uiso 1 1 calc GR . . . .
 H1B H 0.032375 0.097629 0.585705 0.065 Uiso 1 1 calc GR . . . .
 H1C H -0.056800 0.172700 0.612905 0.065 Uiso 1 1 calc GR . . . .
 C23 C 0.2688(2) 0.61361(19) 0.45745(18) 0.0398(6) Uani 1 1 d . . . . .
 H23A H 0.329884 0.622068 0.482923 0.060 Uiso 1 1 calc GR . . . .
 H23B H 0.199532 0.633435 0.485588 0.060 Uiso 1 1 calc GR . . . .
 H23C H 0.268337 0.653092 0.392236 0.060 Uiso 1 1 calc GR . . . .
 C1S C 0.66807(19) 0.18319(18) 0.21780(16) 0.0351(5) Uani 1 1 d . . . . .
 H1S H 0.599294 0.189866 0.254769 0.042 Uiso 1 1 calc R . . . .
 C38 C 0.04534(18) 0.22478(18) 1.14078(14) 0.0349(5) Uani 1 1 d . . . . .
 H38A H -0.023586 0.203167 1.170156 0.042 Uiso 1 1 calc R . . . .
 H38B H 0.044179 0.286586 1.143586 0.042 Uiso 1 1 calc R . . . .
 C37 C 0.1238(2) 0.1359(2) 1.29260(16) 0.0466(7) Uani 1 1 d . . . . .
 H37A H 0.054179 0.114406 1.316103 0.070 Uiso 1 1 calc GR . . . .
 H37B H 0.121168 0.196855 1.296283 0.070 Uiso 1 1 calc GR . . . .
 H37C H 0.183830 0.087372 1.328466 0.070 Uiso 1 1 calc GR . . . .
 C34 C 0.24921(19) 0.18880(19) 1.15953(15) 0.0358(5) Uani 1 1 d . . . . .
 H34A H 0.238872 0.252249 1.161394 0.043 Uiso 1 1 calc R . . . .
 H34B H 0.308327 0.144868 1.200859 0.043 Uiso 1 1 calc R . . . .
 C26 C 0.4934(2) 0.3425(2) 0.65497(18) 0.0417(6) Uani 1 1 d . . . . .
 H26A H 0.455617 0.398022 0.604655 0.063 Uiso 1 1 calc GR . . . .
 H26B H 0.517354 0.288174 0.638186 0.063 Uiso 1 1 calc GR . . . .
 H26C H 0.557446 0.358898 0.668959 0.063 Uiso 1 1 calc GR . . . .
 C50 C 0.1530(2) 0.0335(2) 0.92435(19) 0.0467(6) Uani 1 1 d . . . . .
 H50A H 0.166818 -0.006773 0.988344 0.070 Uiso 1 1 calc GR . . . .
 H50B H 0.190699 -0.001306 0.888374 0.070 Uiso 1 1 calc GR . . . .
 H50C H 0.073999 0.049080 0.915148 0.070 Uiso 1 1 calc GR . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Rb2 O11 2.8135(14) . ?
 Rb2 O10 2.7934(16) . ?
 Rb2 O12 2.8872(16) . ?
 Rb2 O6 2.8786(16) . ?
 Rb2 O9 2.8800(16) . ?
 Rb2 O14 2.7746(17) . ?
 Rb1 O3 2.8780(13) . ?
 Rb1 O2 2.8828(14) . ?
 Rb1 O1 2.9229(16) . ?
 Rb1 O4 2.8018(15) . ?
 Rb1 O12 3.1544(15) . ?
 Rb1 O6 2.7858(19) . ?
 Rb1 O9 3.3463(17) . ?
 Rb1 O16 2.6979(17) . ?
 Cl2S C1S 1.764(3) . ?
 Cl4S C1S 1.761(3) . ?
 Al1 O3 1.8456(15) . ?
 Al1 O2 1.8632(15) . ?
 Al1 O5 1.9103(16) . ?
 Al1 O7 1.8678(15) . ?
 Al1 N1 2.0445(18) . ?
 Al1 N2 2.0900(17) . ?
 Al2 O11 1.8561(15) . ?
 Al2 O15 1.8936(16) . ?
 Al2 O13 1.8720(16) . ?
 Al2 O10 1.8418(15) . ?
 Al2 N4 2.0728(18) . ?
 Al2 N3 2.0450(19) . ?
 Cl3S C1S 1.768(3) . ?
 O3 C20 1.317(2) . ?
 O11 C45 1.312(3) . ?
 O2 C7 1.309(2) . ?
 O15 C49 1.286(3) . ?
 O5 C22 1.281(2) . ?
 O7 C24 1.288(3) . ?
 O1 C2 1.380(3) . ?
 O1 C1 1.429(3) . ?
 O13 C47 1.288(3) . ?
 O10 C32 1.316(2) . ?
 O4 C19 1.366(2) . ?
 O4 C21 1.432(3) . ?
 O12 C44 1.378(3) . ?
 O12 C46 1.437(2) . ?
 O6 C22 1.229(3) . ?
 O9 C27 1.376(3) . ?
 O9 C26 1.432(3) . ?
 O14 C47 1.226(3) . ?
 O8 C24 1.229(3) . ?
 O16 C49 1.225(3) . ?
 N1 C9 1.473(3) . ?
 N1 C8 1.283(3) . ?
 N4 C39 1.277(3) . ?
 N4 C38 1.471(3) . ?
 N2 C14 1.287(3) . ?
 N2 C13 1.471(3) . ?
 N3 C33 1.285(3) . ?
 N3 C34 1.468(3) . ?
 C45 C44 1.409(3) . ?
 C45 C40 1.415(3) . ?
 C20 C15 1.406(3) . ?
 C20 C19 1.424(3) . ?
 C9 C10 1.534(3) . ?
 C7 C2 1.433(3) . ?
 C7 C6 1.412(3) . ?
 C15 C14 1.445(3) . ?
 C15 C16 1.413(3) . ?
 C44 C43 1.383(3) . ?
 C2 C3 1.376(3) . ?
 C24 C25 1.513(3) . ?
 C19 C18 1.383(3) . ?
 C40 C39 1.447(3) . ?
 C40 C41 1.410(3) . ?
 C6 C8 1.448(3) . ?
 C6 C5 1.405(3) . ?
 C47 C48 1.512(3) . ?
 C10 C12 1.536(3) . ?
 C10 C13 1.531(3) . ?
 C10 C11 1.533(3) . ?
 C32 C31 1.401(3) . ?
 C32 C27 1.421(3) . ?
 C31 C33 1.441(3) . ?
 C31 C30 1.419(3) . ?
 C49 C50 1.498(3) . ?
 C41 C42 1.367(4) . ?
 C16 C17 1.373(3) . ?
 C5 C4 1.377(3) . ?
 C22 C23 1.512(3) . ?
 C3 C4 1.401(3) . ?
 C18 C17 1.398(3) . ?
 C30 C29 1.358(4) . ?
 C27 C28 1.389(3) . ?
 C43 C42 1.399(4) . ?
 C35 C36 1.528(4) . ?
 C35 C38 1.540(3) . ?
 C35 C37 1.538(3) . ?
 C35 C34 1.532(4) . ?
 C29 C28 1.397(4) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O11 Rb2 O12 55.38(4) . . ?
 O11 Rb2 O6 123.42(5) . . ?
 O11 Rb2 O9 102.39(4) . . ?
 O10 Rb2 O11 57.17(4) . . ?
 O10 Rb2 O12 101.35(4) . . ?
 O10 Rb2 O6 123.78(5) . . ?
 O10 Rb2 O9 55.55(4) . . ?
 O6 Rb2 O12 72.07(5) . . ?
 O6 Rb2 O9 73.06(5) . . ?
 O9 Rb2 O12 107.69(5) . . ?
 O14 Rb2 O11 73.04(5) . . ?
 O14 Rb2 O10 70.76(5) . . ?
 O14 Rb2 O12 118.84(5) . . ?
 O14 Rb2 O6 161.57(5) . . ?
 O14 Rb2 O9 113.89(5) . . ?
 O3 Rb1 O2 54.45(4) . . ?
 O3 Rb1 O1 100.33(4) . . ?
 O3 Rb1 O12 136.79(4) . . ?
 O3 Rb1 O9 82.31(4) . . ?
 O2 Rb1 O1 54.45(4) . . ?
 O2 Rb1 O12 99.09(4) . . ?
 O2 Rb1 O9 125.86(4) . . ?
 O1 Rb1 O12 84.22(4) . . ?
 O1 Rb1 O9 175.60(4) . . ?
 O4 Rb1 O3 55.44(4) . . ?
 O4 Rb1 O2 100.79(4) . . ?
 O4 Rb1 O1 111.82(5) . . ?
 O4 Rb1 O12 159.43(4) . . ?
 O4 Rb1 O9 72.57(4) . . ?
 O12 Rb1 O9 91.45(4) . . ?
 O6 Rb1 O3 68.87(4) . . ?
 O6 Rb1 O2 67.54(5) . . ?
 O6 Rb1 O1 110.30(5) . . ?
 O6 Rb1 O4 113.95(5) . . ?
 O6 Rb1 O12 69.32(4) . . ?
 O6 Rb1 O9 67.25(5) . . ?
 O16 Rb1 O3 139.29(5) . . ?
 O16 Rb1 O2 163.46(5) . . ?
 O16 Rb1 O1 109.18(5) . . ?
 O16 Rb1 O4 87.19(5) . . ?
 O16 Rb1 O12 75.00(5) . . ?
 O16 Rb1 O6 122.50(5) . . ?
 O16 Rb1 O9 70.26(5) . . ?
 O3 Al1 O2 90.56(6) . . ?
 O3 Al1 O5 94.50(7) . . ?
 O3 Al1 O7 94.55(7) . . ?
 O3 Al1 N1 178.93(8) . . ?
 O3 Al1 N2 89.37(7) . . ?
 O2 Al1 O5 94.57(7) . . ?
 O2 Al1 O7 94.07(7) . . ?
 O2 Al1 N1 89.92(7) . . ?
 O2 Al1 N2 178.71(7) . . ?
 O5 Al1 N1 84.51(7) . . ?
 O5 Al1 N2 86.72(7) . . ?
 O7 Al1 O5 167.42(7) . . ?
 O7 Al1 N1 86.37(7) . . ?
 O7 Al1 N2 84.66(7) . . ?
 N1 Al1 N2 90.17(7) . . ?
 O11 Al2 O15 93.26(7) . . ?
 O11 Al2 O13 93.58(7) . . ?
 O11 Al2 N4 87.96(7) . . ?
 O11 Al2 N3 177.30(8) . . ?
 O15 Al2 N4 83.80(7) . . ?
 O15 Al2 N3 85.43(7) . . ?
 O13 Al2 O15 167.69(7) . . ?
 O13 Al2 N4 86.23(7) . . ?
 O13 Al2 N3 87.30(8) . . ?
 O10 Al2 O11 93.01(7) . . ?
 O10 Al2 O15 94.03(7) . . ?
 O10 Al2 O13 95.81(7) . . ?
 O10 Al2 N4 177.67(8) . . ?
 O10 Al2 N3 89.44(7) . . ?
 N3 Al2 N4 89.55(7) . . ?
 Al1 O3 Rb1 105.82(6) . . ?
 C20 O3 Rb1 123.25(12) . . ?
 C20 O3 Al1 126.85(12) . . ?
 Al2 O11 Rb2 101.99(6) . . ?
 C45 O11 Rb2 126.08(12) . . ?
 C45 O11 Al2 123.73(13) . . ?
 Al1 O2 Rb1 105.13(6) . . ?
 C7 O2 Rb1 125.62(12) . . ?
 C7 O2 Al1 126.92(12) . . ?
 C49 O15 Al2 134.89(14) . . ?
 C22 O5 Al1 134.95(15) . . ?
 C24 O7 Al1 142.74(14) . . ?
 C2 O1 Rb1 124.60(13) . . ?
 C2 O1 C1 116.88(18) . . ?
 C1 O1 Rb1 118.52(14) . . ?
 C47 O13 Al2 138.35(14) . . ?
 Al2 O10 Rb2 103.12(6) . . ?
 C32 O10 Rb2 126.80(13) . . ?
 C32 O10 Al2 124.74(15) . . ?
 C19 O4 Rb1 126.93(13) . . ?
 C19 O4 C21 117.36(17) . . ?
 C21 O4 Rb1 115.69(12) . . ?
 Rb2 O12 Rb1 79.89(4) . . ?
 C44 O12 Rb2 123.41(12) . . ?
 C44 O12 Rb1 110.07(12) . . ?
 C44 O12 C46 116.85(17) . . ?
 C46 O12 Rb2 118.24(14) . . ?
 C46 O12 Rb1 92.10(11) . . ?
 Rb1 O6 Rb2 86.58(5) . . ?
 C22 O6 Rb2 136.60(15) . . ?
 C22 O6 Rb1 136.00(15) . . ?
 Rb2 O9 Rb1 76.80(4) . . ?
 C27 O9 Rb2 123.43(12) . . ?
 C27 O9 Rb1 114.72(13) . . ?
 C27 O9 C26 116.62(19) . . ?
 C26 O9 Rb2 117.29(16) . . ?
 C26 O9 Rb1 94.31(13) . . ?
 C47 O14 Rb2 129.49(16) . . ?
 C49 O16 Rb1 164.48(17) . . ?
 C9 N1 Al1 122.48(13) . . ?
 C8 N1 Al1 122.26(15) . . ?
 C8 N1 C9 115.20(17) . . ?
 C39 N4 Al2 120.55(14) . . ?
 C39 N4 C38 116.45(18) . . ?
 C38 N4 Al2 122.94(15) . . ?
 C14 N2 Al1 119.98(14) . . ?
 C14 N2 C13 114.73(17) . . ?
 C13 N2 Al1 125.18(13) . . ?
 C33 N3 Al2 120.36(16) . . ?
 C33 N3 C34 116.24(19) . . ?
 C34 N3 Al2 123.39(14) . . ?
 O11 C45 C44 120.04(19) . . ?
 O11 C45 C40 122.49(19) . . ?
 C44 C45 C40 117.4(2) . . ?
 O3 C20 C15 122.84(19) . . ?
 O3 C20 C19 119.53(17) . . ?
 C15 C20 C19 117.62(18) . . ?
 N1 C9 C10 114.79(17) . . ?
 O2 C7 C2 120.20(18) . . ?
 O2 C7 C6 123.15(19) . . ?
 C6 C7 C2 116.63(18) . . ?
 C20 C15 C14 121.61(18) . . ?
 C20 C15 C16 120.5(2) . . ?
 C16 C15 C14 117.86(19) . . ?
 O12 C44 C45 114.97(19) . . ?
 O12 C44 C43 123.9(2) . . ?
 C43 C44 C45 121.1(2) . . ?
 O1 C2 C7 114.01(18) . . ?
 C3 C2 O1 124.6(2) . . ?
 C3 C2 C7 121.3(2) . . ?
 O7 C24 C25 117.87(18) . . ?
 O8 C24 O7 122.3(2) . . ?
 O8 C24 C25 119.8(2) . . ?
 O4 C19 C20 114.55(17) . . ?
 O4 C19 C18 124.6(2) . . ?
 C18 C19 C20 120.87(19) . . ?
 N2 C14 C15 127.25(18) . . ?
 C45 C40 C39 121.0(2) . . ?
 C41 C40 C45 120.4(2) . . ?
 C41 C40 C39 118.5(2) . . ?
 N4 C39 C40 125.76(19) . . ?
 C7 C6 C8 121.26(18) . . ?
 C5 C6 C7 121.1(2) . . ?
 C5 C6 C8 117.46(19) . . ?
 O13 C47 C48 113.8(2) . . ?
 O14 C47 O13 126.3(2) . . ?
 O14 C47 C48 120.0(2) . . ?
 N1 C8 C6 126.53(19) . . ?
 C9 C10 C12 112.19(18) . . ?
 C13 C10 C9 109.44(16) . . ?
 C13 C10 C12 111.28(18) . . ?
 C13 C10 C11 107.31(18) . . ?
 C11 C10 C9 106.55(17) . . ?
 C11 C10 C12 109.87(18) . . ?
 O10 C32 C31 122.96(19) . . ?
 O10 C32 C27 119.2(2) . . ?
 C31 C32 C27 117.8(2) . . ?
 C32 C31 C33 121.09(19) . . ?
 C32 C31 C30 120.4(2) . . ?
 C30 C31 C33 118.3(2) . . ?
 O15 C49 C50 114.8(2) . . ?
 O16 C49 O15 125.7(2) . . ?
 O16 C49 C50 119.4(2) . . ?
 C42 C41 C40 120.7(2) . . ?
 N3 C33 C31 126.6(2) . . ?
 C17 C16 C15 120.7(2) . . ?
 C6 C5 Rb2 116.81(14) . 2_566 ?
 C4 C5 Rb2 82.59(13) . 2_566 ?
 C4 C5 C6 120.7(2) . . ?
 O5 C22 C23 116.7(2) . . ?
 O6 C22 O5 125.9(2) . . ?
 O6 C22 C23 117.45(19) . . ?
 C2 C3 C4 120.8(2) . . ?
 C19 C18 C17 120.7(2) . . ?
 N2 C13 C10 114.88(17) . . ?
 C29 C30 C31 120.7(2) . . ?
 C5 C4 Rb2 74.26(13) . 2_566 ?
 C5 C4 C3 119.4(2) . . ?
 C3 C4 Rb2 119.63(15) . 2_566 ?
 O9 C27 C32 114.92(19) . . ?
 O9 C27 C28 124.5(2) . . ?
 C28 C27 C32 120.6(2) . . ?
 C44 C43 C42 120.6(2) . . ?
 C36 C35 C38 110.8(2) . . ?
 C36 C35 C37 109.7(2) . . ?
 C36 C35 C34 111.61(18) . . ?
 C37 C35 C38 107.45(17) . . ?
 C34 C35 C38 110.2(2) . . ?
 C34 C35 C37 106.9(2) . . ?
 C16 C17 C18 119.6(2) . . ?
 C41 C42 C43 119.6(2) . . ?
 C30 C29 C28 120.0(2) . . ?
 C27 C28 C29 120.5(2) . . ?
 Cl2S C1S Cl3S 109.84(13) . . ?
 Cl4S C1S Cl2S 109.77(13) . . ?
 Cl4S C1S Cl3S 109.62(14) . . ?
 N4 C38 C35 113.22(17) . . ?
 N3 C34 C35 113.7(2) . . ?


_ins_header
;
TITL 014RWFK20 in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  12.545975  15.734270  16.451350  64.3717  82.3965  76.6383
ZERR    2.00   0.000257   0.000439   0.000498   0.0029   0.0021   0.0020
LATT  1
SFAC C H N O Al Rb
UNIT 200.00 200.00 4.00 16.00 2.00 2.00
REM  CrysAlisPro recorded range (K): Min=149.9; max=150.0; aver:150.0
TEMP -123
TREF
HKLF 4
END
;
_olex2_submission_special_instructions  'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max  1.270
_oxdiff_exptl_absorpt_empirical_full_min  0.764

data_016rwfk20
_audit_creation_date               2020-12-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      '12 Mansfield Road, OX1 3TA'
_audit_contact_author_email        'Charlotte.Williams@chem.ox.ac.uk'
_audit_contact_author_name         'Charlotte Williams'
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           'C25 H30 Al Cs N2 O8, C H Cl3'
_chemical_formula_sum              'C26 H31 Al Cl3 Cs N2 O8'
_chemical_formula_weight           765.77
_chemical_melting_point            ?
_chemical_oxdiff_formula           C25H33Al1Cs1N2O8
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Al' 'Al' 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cs' 'Cs' -0.7457 7.9052
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        monoclinic
_space_group_IT_number             14
_space_group_name_H-M_alt          'P 1 21/c 1'
_space_group_name_Hall             '-P 2ybc'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'

_cell_length_a                     14.9518(2)
_cell_length_b                     12.88710(10)
_cell_length_c                     16.7675(2)
_cell_angle_alpha                  90
_cell_angle_beta                   98.5770(10)
_cell_angle_gamma                  90
_cell_volume                       3194.72(6)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      10406
_cell_measurement_temperature      150.01(10)
_cell_measurement_theta_max        76.9830
_cell_measurement_theta_min        2.9950
_shelx_estimated_absorpt_T_max     0.222
_shelx_estimated_absorpt_T_min     0.146
_exptl_absorpt_coefficient_mu      12.029
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.66956
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              'clear light colourless'
_exptl_crystal_colour_lustre       clear
_exptl_crystal_colour_modifier     light
_exptl_crystal_colour_primary      colourless
_exptl_crystal_density_diffrn      1.592
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               1536
_exptl_crystal_recrystallization_method  ?
_exptl_crystal_size_max            0.26
_exptl_crystal_size_mid            0.18
_exptl_crystal_size_min            0.179
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0277
_diffrn_reflns_av_unetI/netI       0.0305
_diffrn_reflns_Laue_measured_fraction_full  1.000
_diffrn_reflns_Laue_measured_fraction_max  0.987
_diffrn_reflns_limit_h_max         18
_diffrn_reflns_limit_h_min         -16
_diffrn_reflns_limit_k_max         15
_diffrn_reflns_limit_k_min         -16
_diffrn_reflns_limit_l_max         21
_diffrn_reflns_limit_l_min         -18
_diffrn_reflns_number              15348
_diffrn_reflns_point_group_measured_fraction_full  1.000
_diffrn_reflns_point_group_measured_fraction_max  0.987
_diffrn_reflns_theta_full          67.684
_diffrn_reflns_theta_max           76.851
_diffrn_reflns_theta_min           2.989
_diffrn_ambient_environment        N~2~
_diffrn_ambient_temperature        150.01(10)
_diffrn_detector                   'CCD plate'
_diffrn_detector_area_resol_mean   10.5035
_diffrn_detector_type              Atlas
_diffrn_measured_fraction_theta_full  1.000
_diffrn_measured_fraction_theta_max  0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -99.00 -43.00   1.00    1.00    --    0.00-178.00  30.00   56
  2  ω    -77.00 -43.00   1.00    1.00    --    0.00 178.00-150.00   34
  3  ω     -3.00  33.00   1.00    2.00    --  -60.50  15.00 120.00   36
  4  ω     -3.00  32.00   1.00    2.00    --  -60.50  15.00 -90.00   35
  5  ω   -150.00-111.00   1.00    2.00    --  -60.50 -94.00 -90.00   39
  6  ω      4.00  31.00   1.00    2.00    --  -60.50  15.00-150.00   27
  7  ω     -1.00  28.00   1.00    2.00    --  -60.50  15.00-120.00   29
  8  ω    -14.00  22.00   1.00    2.00    --  -60.50  30.00   0.00   36
  9  ω     -3.00  32.00   1.00    2.00    --  -60.50  15.00 -30.00   35
 10  ω     99.00 149.00   1.00    2.00    --   60.50 125.00-150.00   50
 11  ω     99.00 133.00   1.00    2.00    --   60.50 125.00  60.00   34
 12  ω    109.00 146.00   1.00    2.00    --   60.50 125.00   0.00   37
 13  ω    103.00 167.00   1.00    4.00    --  121.00  77.00  60.00   64
 14  ω     76.00 102.00   1.00    4.00    --  121.00 -91.00  90.00   26
 15  ω     26.00  52.00   1.00    4.00    --  121.00 -91.00  90.00   26
 16  ω    115.00 162.00   1.00    4.00    --  121.00  63.00  90.00   47
 17  ω    103.00 178.00   1.00    4.00    --  121.00  77.00 -60.00   75
 18  ω    114.00 177.00   1.00    4.00    --  121.00  77.00 -90.00   63
 19  ω     48.00  76.00   1.00    4.00    --  121.00 -50.00  60.00   28
 20  ω    105.00 177.00   1.00    4.00    --  121.00  77.00   0.00   72
 21  ω     42.00  96.00   1.00    4.00    --  121.00 -63.00-120.00   54
 22  ω     89.00 120.00   1.00    4.00    --  121.00  50.00   0.00   31
 23  ω     40.00  78.00   1.00    4.00    --  121.00 -50.00 -90.00   38
 24  ω     84.00 177.00   1.00    4.00    --  121.00  63.00  30.00   93
 25  ω     80.00 106.00   1.00    4.00    --  121.00  63.00  90.00   26
 26  ω     45.00  80.00   1.00    1.00    --    0.00  19.00 -60.00   35
 27  ω      2.00  39.00   1.00    1.00    --    0.00 -77.00  90.00   37
 28  ω    -63.00 -38.00   1.00    1.00    --    0.00 178.00-150.00   25
 29  ω      2.00  34.00   1.00    1.00    --    0.00  19.00 -60.00   32
 30  ω     -2.00  24.00   1.00    2.00    --  -60.50  30.00-120.00   26
 31  ω    -14.00   8.00   1.00    2.00    --  -60.50  30.00-150.00   22
;
_diffrn_measurement_device         'four-circle diffractometer'
_diffrn_measurement_device_type    'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_type        
 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11        -0.1006973000
_diffrn_orient_matrix_UB_12        0.0240226000
_diffrn_orient_matrix_UB_13        -0.0284345000
_diffrn_orient_matrix_UB_21        -0.0022565000
_diffrn_orient_matrix_UB_22        -0.0824486000
_diffrn_orient_matrix_UB_23        -0.0667852000
_diffrn_orient_matrix_UB_31        -0.0268623000
_diffrn_orient_matrix_UB_32        -0.0831125000
_diffrn_orient_matrix_UB_33        0.0580133000
_diffrn_radiation_monochromator    mirror
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             CuK\a
_diffrn_radiation_wavelength       1.54184
_diffrn_source                     'micro-focus sealed X-ray tube'
_diffrn_source_type                'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  6283
_reflns_number_total               6656
_reflns_odcompleteness_completeness  99.94
_reflns_odcompleteness_iscentric   1
_reflns_odcompleteness_theta       74.33
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_collection         'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_reduction          'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.697
_refine_diff_density_min           -1.290
_refine_diff_density_rms           0.076
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.046
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       404
_refine_ls_number_reflns           6656
_refine_ls_number_restraints       3
_refine_ls_R_factor_all            0.0301
_refine_ls_R_factor_gt             0.0280
_refine_ls_restrained_S_all        1.049
_refine_ls_shift/su_max            0.002
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0392P)²+1.6830P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0712
_refine_ls_wR_factor_ref           0.0727
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl2S-C1S \\sim Cl2T-C1S
 with sigma of 0.02
 Cl4S-C1S \\sim Cl4T-C1S
 with sigma of 0.02
 Cl3S-C1S \\sim Cl3T-C1S
 with sigma of 0.02
3. Others
 Sof(H1SA)=Sof(Cl2T)=Sof(Cl4T)=Sof(Cl3T)=1-FVAR(1)
 Sof(Cl2S)=Sof(Cl4S)=Sof(Cl3S)=Sof(H1S)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C1S(H1SA), C1S(H1S)
4.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C9(H9A,H9B)
4.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C8(H8), C16(H16), C18(H18), C5(H5), C3(H3), C17(H17), C4(H4)
4.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C25(H25A,H25B,H25C), C21(H21A,H21B,
 H21C), C1(H1A,H1B,H1C), C23(H23A,H23B,H23C)
;
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Cs1 Cs 0.74859(2) 0.18570(2) 0.95263(2) 0.02322(6) Uani 1 1 d . . . . .
 Cl2S Cl 0.45789(14) 0.37286(16) 0.51223(18) 0.0207(6) Uani 0.628(15) 1 d D . P A
 1
 Al1 Al 0.84825(4) 0.33007(5) 0.77542(4) 0.01306(12) Uani 1 1 d . . . . .
 Cl4S Cl 0.26823(17) 0.39737(18) 0.52892(14) 0.0263(7) Uani 0.628(15) 1 d D . P A
 1
 Cl3S Cl 0.31689(16) 0.2905(2) 0.39106(18) 0.0529(9) Uani 0.628(15) 1 d D . P A 1
 O3 O 0.79975(11) 0.19920(12) 0.78190(9) 0.0173(3) Uani 1 1 d . . . . .
 O7 O 0.75808(10) 0.36946(12) 0.68782(9) 0.0172(3) Uani 1 1 d . . . . .
 O2 O 0.78354(10) 0.37756(12) 0.85328(9) 0.0186(3) Uani 1 1 d . . . . .
 O5 O 0.95615(11) 0.30527(13) 0.84498(10) 0.0205(3) Uani 1 1 d . . . . .
 O8 O 0.64422(11) 0.37545(16) 0.58828(10) 0.0279(4) Uani 1 1 d . . . . .
 O4 O 0.66853(12) 0.06710(15) 0.79764(11) 0.0297(4) Uani 1 1 d . . . . .
 O1 O 0.63656(12) 0.38188(14) 0.92093(11) 0.0276(4) Uani 1 1 d . . . . .
 N2 N 0.91845(12) 0.27800(14) 0.68758(10) 0.0152(3) Uani 1 1 d . . . . .
 O6 O 0.93866(13) 0.24602(19) 0.96646(11) 0.0374(5) Uani 1 1 d . . . . .
 N1 N 0.89779(12) 0.47834(15) 0.76533(10) 0.0168(3) Uani 1 1 d . . . . .
 C20 C 0.77546(14) 0.13459(16) 0.72187(13) 0.0169(4) Uani 1 1 d . . . . .
 C14 C 0.89189(15) 0.19984(17) 0.64272(13) 0.0172(4) Uani 1 1 d . . . . .
 H14 H 0.924848 0.184651 0.599893 0.021 Uiso 1 1 calc R . . . .
 C22 C 0.98357(16) 0.28483(19) 0.91895(14) 0.0213(4) Uani 1 1 d . . . . .
 C6 C 0.77132(16) 0.55786(18) 0.81909(14) 0.0228(5) Uani 1 1 d . . . . .
 C15 C 0.81629(15) 0.13276(17) 0.65146(13) 0.0177(4) Uani 1 1 d . . . . .
 C10 C 0.99980(14) 0.44374(17) 0.66113(12) 0.0174(4) Uani 1 1 d . . . . .
 C8 C 0.85418(16) 0.55812(17) 0.78364(13) 0.0214(4) Uani 1 1 d . . . . .
 H8 H 0.878375 0.623990 0.772989 0.026 Uiso 1 1 calc R . . . .
 C7 C 0.74111(15) 0.46657(18) 0.85269(13) 0.0187(4) Uani 1 1 d . . . . .
 C11 C 0.92555(15) 0.47399(18) 0.59232(13) 0.0209(4) Uani 1 1 d . . . . .
 H11A H 0.936230 0.439207 0.542624 0.031 Uiso 1 1 calc GR . . . .
 H11B H 0.926199 0.549331 0.584502 0.031 Uiso 1 1 calc GR . . . .
 H11C H 0.866602 0.452834 0.605686 0.031 Uiso 1 1 calc GR . . . .
 C19 C 0.70646(16) 0.05993(19) 0.72818(14) 0.0233(5) Uani 1 1 d . . . . .
 C13 C 1.00372(15) 0.32597(18) 0.67305(14) 0.0190(4) Uani 1 1 d . . . . .
 H13A H 1.022375 0.293799 0.624502 0.023 Uiso 1 1 calc R . . . .
 H13B H 1.050977 0.309960 0.719310 0.023 Uiso 1 1 calc R . . . .
 C9 C 0.98622(15) 0.49885(18) 0.73968(13) 0.0201(4) Uani 1 1 d . . . . .
 H9A H 1.034593 0.476533 0.783163 0.024 Uiso 1 1 calc R . . . .
 H9B H 0.992705 0.574568 0.732371 0.024 Uiso 1 1 calc R . . . .
 C12 C 1.09239(16) 0.4766(2) 0.64098(15) 0.0263(5) Uani 1 1 d . . . . .
 H12A H 1.102722 0.443455 0.590555 0.039 Uiso 1 1 calc GR . . . .
 H12B H 1.139778 0.455238 0.684700 0.039 Uiso 1 1 calc GR . . . .
 H12C H 1.093868 0.552194 0.634805 0.039 Uiso 1 1 calc GR . . . .
 C24 C 0.67515(14) 0.35446(16) 0.65922(13) 0.0163(4) Uani 1 1 d . . . . .
 C25 C 0.61106(16) 0.3137(2) 0.71384(16) 0.0265(5) Uani 1 1 d . . . . .
 H25A H 0.570757 0.261778 0.684753 0.040 Uiso 1 1 calc GR . . . .
 H25B H 0.575017 0.371117 0.730411 0.040 Uiso 1 1 calc GR . . . .
 H25C H 0.645936 0.281711 0.761687 0.040 Uiso 1 1 calc GR . . . .
 C2 C 0.66124(16) 0.4738(2) 0.88919(14) 0.0232(5) Uani 1 1 d . . . . .
 C16 C 0.79111(17) 0.05749(19) 0.59119(15) 0.0262(5) Uani 1 1 d . . . . .
 H16 H 0.819566 0.056753 0.544174 0.031 Uiso 1 1 calc R . . . .
 C18 C 0.68322(18) -0.0134(2) 0.66847(16) 0.0308(5) Uani 1 1 d . . . . .
 H18 H 0.637857 -0.063339 0.674106 0.037 Uiso 1 1 calc R . . . .
 C5 C 0.7253(2) 0.6523(2) 0.82385(17) 0.0309(5) Uani 1 1 d . . . . .
 H5 H 0.748160 0.713871 0.803127 0.037 Uiso 1 1 calc R . . . .
 C3 C 0.61510(18) 0.5664(2) 0.89094(16) 0.0301(5) Uani 1 1 d . . . . .
 H3 H 0.561165 0.568915 0.914502 0.036 Uiso 1 1 calc R . . . .
 C17 C 0.72601(19) -0.0144(2) 0.59998(17) 0.0332(6) Uani 1 1 d . . . . .
 H17 H 0.709883 -0.065273 0.559341 0.040 Uiso 1 1 calc R . . . .
 C21 C 0.5879(2) 0.0086(3) 0.80025(19) 0.0462(8) Uani 1 1 d . . . . .
 H21A H 0.602352 -0.065567 0.802400 0.069 Uiso 1 1 calc GR . . . .
 H21B H 0.544335 0.023233 0.751855 0.069 Uiso 1 1 calc GR . . . .
 H21C H 0.561649 0.028155 0.848295 0.069 Uiso 1 1 calc GR . . . .
 C4 C 0.6470(2) 0.6563(2) 0.85845(18) 0.0348(6) Uani 1 1 d . . . . .
 H4 H 0.615153 0.719865 0.860057 0.042 Uiso 1 1 calc R . . . .
 C1S C 0.3477(2) 0.3938(2) 0.45919(17) 0.0351(6) Uani 1 1 d D . . . .
 H1SA H 0.346797 0.467305 0.439961 0.042 Uiso 0.372(15) 1 calc R . P A 2
 H1S H 0.345853 0.460874 0.428994 0.042 Uiso 0.628(15) 1 calc R . P A 1
 C1 C 0.55987(19) 0.3832(2) 0.9624(2) 0.0400(7) Uani 1 1 d . . . . .
 H1A H 0.551443 0.314128 0.984665 0.060 Uiso 1 1 calc GR . . . .
 H1B H 0.505845 0.402262 0.924709 0.060 Uiso 1 1 calc GR . . . .
 H1C H 0.569648 0.433948 1.006347 0.060 Uiso 1 1 calc GR . . . .
 C23 C 1.0823(2) 0.3082(3) 0.9467(2) 0.0542(10) Uani 1 1 d . . . . .
 H23A H 1.116023 0.300821 0.901186 0.081 Uiso 1 1 calc GR . . . .
 H23B H 1.106362 0.259680 0.989550 0.081 Uiso 1 1 calc GR . . . .
 H23C H 1.088567 0.379421 0.967347 0.081 Uiso 1 1 calc GR . . . .
 Cl2T Cl 0.4561(5) 0.3724(6) 0.5060(5) 0.067(2) Uani 0.372(15) 1 d D . P A 2
 Cl4T Cl 0.2706(5) 0.3884(8) 0.5227(5) 0.088(3) Uani 0.372(15) 1 d D . P A 2
 Cl3T Cl 0.3238(8) 0.3195(13) 0.3733(6) 0.148(4) Uani 0.372(15) 1 d D . P A 2


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Cs1 O3 3.0763(15) . ?
 Cs1 O2 3.0694(15) . ?
 Cs1 O8 3.0478(17) 4_566 ?
 Cs1 O4 3.0975(18) . ?
 Cs1 O1 3.0356(18) . ?
 Cs1 O6 2.9220(19) . ?
 Cl2S C1S 1.773(4) . ?
 Al1 O3 1.8453(16) . ?
 Al1 O7 1.9084(16) . ?
 Al1 O2 1.8417(16) . ?
 Al1 O5 1.8719(17) . ?
 Al1 N2 2.0451(19) . ?
 Al1 N1 2.065(2) . ?
 Cl4S C1S 1.787(4) . ?
 Cl3S C1S 1.770(4) . ?
 O3 C20 1.315(3) . ?
 O7 C24 1.276(3) . ?
 O2 C7 1.310(3) . ?
 O5 C22 1.274(3) . ?
 O8 C24 1.240(3) . ?
 O4 C19 1.372(3) . ?
 O4 C21 1.428(3) . ?
 O1 C2 1.372(3) . ?
 O1 C1 1.427(3) . ?
 N2 C14 1.284(3) . ?
 N2 C13 1.470(3) . ?
 O6 C22 1.223(3) . ?
 N1 C8 1.279(3) . ?
 N1 C9 1.474(3) . ?
 C20 C15 1.408(3) . ?
 C20 C19 1.426(3) . ?
 C14 C15 1.448(3) . ?
 C22 C23 1.511(4) . ?
 C6 C8 1.452(3) . ?
 C6 C7 1.408(3) . ?
 C6 C5 1.406(3) . ?
 C15 C16 1.411(3) . ?
 C10 C11 1.528(3) . ?
 C10 C13 1.531(3) . ?
 C10 C9 1.536(3) . ?
 C10 C12 1.533(3) . ?
 C7 C2 1.424(3) . ?
 C19 C18 1.383(4) . ?
 C24 C25 1.515(3) . ?
 C2 C3 1.381(3) . ?
 C16 C17 1.368(4) . ?
 C18 C17 1.396(4) . ?
 C5 C4 1.383(4) . ?
 C3 C4 1.394(4) . ?
 C1S Cl2T 1.715(8) . ?
 C1S Cl4T 1.683(8) . ?
 C1S Cl3T 1.722(7) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 O3 Cs1 O4 50.64(4) . . ?
 O2 Cs1 O3 50.45(4) . . ?
 O2 Cs1 O4 91.03(4) . . ?
 O8 Cs1 O3 159.25(4) 4_566 . ?
 O8 Cs1 O2 139.54(5) 4_566 . ?
 O8 Cs1 O4 108.77(5) 4_566 . ?
 O1 Cs1 O3 89.85(4) . . ?
 O1 Cs1 O2 50.82(4) . . ?
 O1 Cs1 O8 90.88(5) . 4_566 ?
 O1 Cs1 O4 97.47(5) . . ?
 O6 Cs1 O3 71.64(5) . . ?
 O6 Cs1 O2 65.57(5) . . ?
 O6 Cs1 O8 127.57(5) . 4_566 ?
 O6 Cs1 O4 116.58(5) . . ?
 O6 Cs1 O1 107.28(6) . . ?
 O3 Al1 O7 92.85(7) . . ?
 O3 Al1 O5 96.72(8) . . ?
 O3 Al1 N2 89.48(7) . . ?
 O3 Al1 N1 177.71(8) . . ?
 O7 Al1 N2 84.98(7) . . ?
 O7 Al1 N1 84.94(7) . . ?
 O2 Al1 O3 90.54(7) . . ?
 O2 Al1 O7 94.11(7) . . ?
 O2 Al1 O5 96.32(7) . . ?
 O2 Al1 N2 179.09(8) . . ?
 O2 Al1 N1 89.04(7) . . ?
 O5 Al1 O7 165.76(7) . . ?
 O5 Al1 N2 84.58(7) . . ?
 O5 Al1 N1 85.56(8) . . ?
 N2 Al1 N1 90.90(8) . . ?
 C1S Cl4S Cs1 97.99(13) . 2_656 ?
 Al1 O3 Cs1 105.12(6) . . ?
 C20 O3 Cs1 126.71(13) . . ?
 C20 O3 Al1 126.85(14) . . ?
 C24 O7 Al1 141.67(14) . . ?
 Al1 O2 Cs1 105.48(7) . . ?
 C7 O2 Cs1 126.01(13) . . ?
 C7 O2 Al1 126.20(14) . . ?
 C22 O5 Al1 139.82(16) . . ?
 C24 O8 Cs1 120.02(14) . 4_565 ?
 C19 O4 Cs1 126.03(13) . . ?
 C19 O4 C21 116.6(2) . . ?
 C21 O4 Cs1 117.20(17) . . ?
 C2 O1 Cs1 127.88(13) . . ?
 C2 O1 C1 117.5(2) . . ?
 C1 O1 Cs1 112.75(17) . . ?
 C14 N2 Al1 122.14(15) . . ?
 C14 N2 C13 115.67(18) . . ?
 C13 N2 Al1 122.17(14) . . ?
 C22 O6 Cs1 132.78(16) . . ?
 C8 N1 Al1 121.47(15) . . ?
 C8 N1 C9 115.94(19) . . ?
 C9 N1 Al1 122.55(15) . . ?
 O3 C20 C15 123.2(2) . . ?
 O3 C20 C19 119.4(2) . . ?
 C15 C20 C19 117.4(2) . . ?
 N2 C14 Cs1 105.61(13) . 4_565 ?
 N2 C14 C15 126.0(2) . . ?
 C15 C14 Cs1 88.06(12) . 4_565 ?
 O5 C22 C23 114.6(2) . . ?
 O6 C22 O5 126.2(2) . . ?
 O6 C22 C23 119.2(2) . . ?
 C7 C6 C8 120.7(2) . . ?
 C5 C6 C8 118.4(2) . . ?
 C5 C6 C7 120.8(2) . . ?
 C20 C15 C14 121.17(19) . . ?
 C20 C15 C16 120.6(2) . . ?
 C16 C15 C14 117.8(2) . . ?
 C11 C10 C13 111.16(18) . . ?
 C11 C10 C9 110.83(19) . . ?
 C11 C10 C12 109.96(18) . . ?
 C13 C10 C9 110.72(18) . . ?
 C13 C10 C12 106.53(19) . . ?
 C12 C10 C9 107.48(18) . . ?
 N1 C8 C6 126.4(2) . . ?
 O2 C7 C6 123.4(2) . . ?
 O2 C7 C2 119.4(2) . . ?
 C6 C7 C2 117.2(2) . . ?
 C10 C11 Cs1 132.69(14) . 4_565 ?
 O4 C19 C20 114.4(2) . . ?
 O4 C19 C18 124.7(2) . . ?
 C18 C19 C20 120.9(2) . . ?
 N2 C13 C10 114.93(18) . . ?
 N1 C9 C10 113.97(17) . . ?
 O7 C24 Cs1 88.09(12) . 4_565 ?
 O7 C24 C25 119.50(19) . . ?
 O8 C24 Cs1 43.66(11) . 4_565 ?
 O8 C24 O7 122.0(2) . . ?
 O8 C24 C25 118.5(2) . . ?
 C25 C24 Cs1 142.56(15) . 4_565 ?
 O1 C2 C7 113.7(2) . . ?
 O1 C2 C3 125.0(2) . . ?
 C3 C2 C7 121.3(2) . . ?
 C17 C16 C15 120.5(2) . . ?
 C19 C18 C17 120.4(2) . . ?
 C4 C5 C6 120.5(3) . . ?
 C2 C3 C4 120.6(2) . . ?
 C16 C17 C18 120.2(2) . . ?
 C5 C4 C3 119.6(2) . . ?
 Cl2S C1S Cl4S 109.5(2) . . ?
 Cl3S C1S Cl2S 109.99(19) . . ?
 Cl3S C1S Cl4S 107.90(19) . . ?
 Cl2T C1S Cl3T 111.0(5) . . ?
 Cl4T C1S Cl2T 113.2(5) . . ?
 Cl4T C1S Cl3T 115.5(6) . . ?
 C1S Cl4T Cs1 95.5(4) . 2_656 ?


_ins_header
;
TITL 016RWFK20 in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184  14.951813  12.887117  16.767502  90.0000  98.5772  90.0000
ZERR    5.00   0.000167   0.000135   0.000183   0.0000   0.0010   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H N O Al Cs
UNIT 125.00 165.00 10.00 40.00 5.00 5.00
REM  CrysAlisPro recorded range (K): Min=150.0; max=150.0; aver:150.0
TEMP -123
TREF
HKLF 4
END
;
_olex2_submission_original_sample_id  016RWFK20
_olex2_submission_special_instructions  'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max  1.303
_oxdiff_exptl_absorpt_empirical_full_min  0.786

data_021rwfk21
_audit_creation_date               2021-07-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      '12 Mansfield Road, OX1 3TA'
_audit_contact_author_email        'Charlotte.Williams@chem.ox.ac.uk'
_audit_contact_author_name         'Charlotte Williams'
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           'C74 H76 Al2 K2 N4 O17'
_chemical_formula_sum              'C74 H76 Al2 K2 N4 O17'
_chemical_formula_weight           1425.54
_chemical_melting_point            ?
_chemical_oxdiff_formula           C100H100Al1K1N4O10
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Al' 'Al' 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'K' 'K' 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        monoclinic
_space_group_IT_number             14
_space_group_name_H-M_alt          'P 1 21/n 1'
_space_group_name_Hall             '-P 2yn'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                     15.0779(2)
_cell_length_b                     30.1479(4)
_cell_length_c                     17.5249(3)
_cell_angle_alpha                  90
_cell_angle_beta                   114.699(2)
_cell_angle_gamma                  90
_cell_volume                       7237.5(2)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      12650
_cell_measurement_temperature      150.00(13)
_cell_measurement_theta_max        75.7420
_cell_measurement_theta_min        3.0970
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      1.979
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.77784
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              'dull yellow'
_exptl_crystal_colour_lustre       dull
_exptl_crystal_colour_primary      yellow
_exptl_crystal_density_diffrn      1.308
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         needle
_exptl_crystal_F_000               2992
_exptl_crystal_size_max            0.49
_exptl_crystal_size_mid            0.128
_exptl_crystal_size_min            0.065
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0513
_diffrn_reflns_av_unetI/netI       0.0550
_diffrn_reflns_Laue_measured_fraction_full  0.998
_diffrn_reflns_Laue_measured_fraction_max  0.987
_diffrn_reflns_limit_h_max         18
_diffrn_reflns_limit_h_min         -12
_diffrn_reflns_limit_k_max         36
_diffrn_reflns_limit_k_min         -37
_diffrn_reflns_limit_l_max         22
_diffrn_reflns_limit_l_min         -22
_diffrn_reflns_number              44644
_diffrn_reflns_point_group_measured_fraction_full  0.998
_diffrn_reflns_point_group_measured_fraction_max  0.987
_diffrn_reflns_theta_full          67.684
_diffrn_reflns_theta_max           76.190
_diffrn_reflns_theta_min           3.139
_diffrn_ambient_environment        N~2~
_diffrn_ambient_temperature        150.00(13)
_diffrn_detector                   'CCD plate'
_diffrn_detector_area_resol_mean   10.4102
_diffrn_detector_type              Atlas
_diffrn_measured_fraction_theta_full  0.998
_diffrn_measured_fraction_theta_max  0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -39.00  12.00   1.00    8.00    --  -42.66  57.00-120.00   51
  2  ω      0.00  27.00   1.00    8.00    --  -42.66  19.00-150.00   27
  3  ω     -1.00  31.00   1.00    8.00    --  -42.66  19.00 -30.00   32
  4  ω     -3.00  35.00   1.00    8.00    --  -42.66  19.00 120.00   38
  5  ω     -5.00  30.00   1.00    8.00    --  -42.66  19.00-180.00   35
  6  ω     76.00 129.00   1.00    8.00    --   42.66 178.00 -90.00   53
  7  ω     92.00 164.00   1.00   30.00    --  111.00  45.00 -30.00   72
  8  ω     60.00 106.00   1.00   30.00    --  111.00 -95.00 120.00   46
  9  ω     40.00  69.00   1.00   30.00    --  111.00 -45.00-150.00   29
 10  ω     42.00  68.00   1.00   30.00    --  111.00 -45.00 -60.00   26
 11  ω     55.00  81.00   1.00   30.00    --  111.00 -61.00-180.00   26
 12  ω     41.00  71.00   1.00   30.00    --  111.00 -45.00  30.00   30
 13  ω    150.00 176.00   1.00   30.00    --  111.00 125.00  30.00   26
 14  ω     33.00  73.00   1.00   30.00    --  111.00 -95.00-150.00   40
 15  ω    106.00 153.00   1.00   30.00    --  111.00 125.00-120.00   47
 16  ω     75.00 101.00   1.00   30.00    --  111.00 -95.00-150.00   26
 17  ω     40.00  70.00   1.00   30.00    --  111.00 -45.00 -90.00   30
 18  ω     87.00 177.00   1.00   30.00    --  111.00  45.00 -60.00   90
 19  ω     48.00 107.00   1.00   30.00    --  111.00-120.00 131.00   59
 20  ω     58.00  91.00   1.00   30.00    --  111.00 -61.00 120.00   33
 21  ω     39.00  84.00   1.00   30.00    --  111.00 -95.00 150.00   45
 22  ω     90.00 167.00   1.00   30.00    --  111.00  45.00  60.00   77
 23  ω     83.00 109.00   1.00   30.00    --  111.00-114.00-155.61   26
 24  ω     42.00  67.00   1.00   30.00    --  111.00-114.00-155.61   25
 25  ω    -21.00 -19.00   1.00    8.00    --  -42.66  38.00  30.00    2
;
_diffrn_measurement_device         'four-circle diffractometer'
_diffrn_measurement_device_type    'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_type        
 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11        -0.0052235000
_diffrn_orient_matrix_UB_12        0.0504429000
_diffrn_orient_matrix_UB_13        0.0116686000
_diffrn_orient_matrix_UB_21        0.0567223000
_diffrn_orient_matrix_UB_22        -0.0056478000
_diffrn_orient_matrix_UB_23        0.0956786000
_diffrn_orient_matrix_UB_31        0.0969631000
_diffrn_orient_matrix_UB_32        0.0060150000
_diffrn_orient_matrix_UB_33        -0.0084180000
_diffrn_radiation_monochromator    mirror
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             CuK\a
_diffrn_radiation_wavelength       1.54184
_diffrn_source                     'micro-focus sealed X-ray tube'
_diffrn_source_type                'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  11897
_reflns_number_total               14927
_reflns_odcompleteness_completeness  99.56
_reflns_odcompleteness_iscentric   1
_reflns_odcompleteness_theta       74.33
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection         'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction          'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.582
_refine_diff_density_min           -0.285
_refine_diff_density_rms           0.052
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.023
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       900
_refine_ls_number_reflns           14927
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0561
_refine_ls_R_factor_gt             0.0428
_refine_ls_restrained_S_all        1.023
_refine_ls_shift/su_max            0.001
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0506P)²+1.0925P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1061
_refine_ls_wR_factor_ref           0.1144
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C44(H44A,H44B), C48(H48A,H48B), C13(H13A,H13B), C73(H73A,H73B),
 C72(H72A,H72B), C74(H74A,H74B), C71(H71A,H71B)
2.b Aromatic/amide H refined with riding coordinates:
 C49(H49), C70(H70), C24(H24), C43(H43), C14(H14), C8(H8), C38(H38), C31(H31),
 C51(H51), C53(H53), C28(H28), C25(H25), C66(H66), C52(H52), C26(H26), C68(H68),
  C59(H59), C39(H39), C32(H32), C16(H16), C67(H67), C69(H69), C40(H40),
 C27(H27), C5(H5), C35(H35), C17(H17), C18(H18), C33(H33), C63(H63), C34(H34),
 C3(H3), C4(H4), C61(H61), C60(H60), C62(H62)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C47(H47A,H47B,H47C), C36(H36A,H36B,H36C), C12(H12A,H12B,
 H12C), C56(H56A,H56B,H56C), C46(H46A,H46B,H46C), C21(H21A,H21B,H21C), C1(H1A,
 H1B,H1C)
;
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 K2 K 0.36012(3) 0.24649(2) 0.63438(2) 0.02918(9) Uani 1 1 d . . . . .
 K1 K 0.34504(3) 0.36994(2) 0.67066(3) 0.03323(10) Uani 1 1 d . . . . .
 Al2 Al 0.40918(4) 0.26626(2) 0.45141(3) 0.02168(11) Uani 1 1 d . . . . .
 Al1 Al 0.28544(4) 0.38701(2) 0.84711(3) 0.02299(11) Uani 1 1 d . . . . .
 O10 O 0.48278(9) 0.27371(4) 0.56475(8) 0.0249(2) Uani 1 1 d . . . . .
 O11 O 0.29557(9) 0.26330(4) 0.46668(8) 0.0253(3) Uani 1 1 d . . . . .
 O13 O 0.39282(9) 0.32855(4) 0.42828(8) 0.0248(2) Uani 1 1 d . . . . .
 O15 O 0.42251(9) 0.20365(4) 0.45161(8) 0.0266(3) Uani 1 1 d . . . . .
 O7 O 0.24878(9) 0.44658(5) 0.84667(8) 0.0278(3) Uani 1 1 d . . . . .
 O9 O 0.51838(10) 0.30294(5) 0.71682(8) 0.0297(3) Uani 1 1 d . . . . .
 O3 O 0.39739(9) 0.39611(5) 0.83188(8) 0.0278(3) Uani 1 1 d . . . . .
 O2 O 0.21289(9) 0.38225(5) 0.73224(8) 0.0290(3) Uani 1 1 d . . . . .
 O5 O 0.31113(9) 0.32517(4) 0.86679(8) 0.0272(3) Uani 1 1 d . . . . .
 O6 O 0.31800(10) 0.29368(5) 0.75336(9) 0.0314(3) Uani 1 1 d . . . . .
 O12 O 0.18102(10) 0.28825(5) 0.53836(8) 0.0305(3) Uani 1 1 d . . . . .
 O16 O 0.43454(12) 0.18105(5) 0.57788(9) 0.0348(3) Uani 1 1 d . . . . .
 O14 O 0.38219(12) 0.36409(5) 0.53701(9) 0.0381(3) Uani 1 1 d . . . . .
 O1 O 0.16842(11) 0.41248(6) 0.57953(9) 0.0410(4) Uani 1 1 d . . . . .
 O4 O 0.50098(12) 0.42631(5) 0.75350(11) 0.0400(3) Uani 1 1 d . . . . .
 N3 N 0.53330(11) 0.27092(5) 0.43238(9) 0.0246(3) Uani 1 1 d . . . . .
 N1 N 0.16060(11) 0.37218(5) 0.86312(10) 0.0264(3) Uani 1 1 d . . . . .
 N4 N 0.32927(11) 0.25990(5) 0.32273(9) 0.0251(3) Uani 1 1 d . . . . .
 N2 N 0.36301(11) 0.39419(5) 0.97484(10) 0.0249(3) Uani 1 1 d . . . . .
 O17 O 0.22487(14) 0.16780(7) 0.63788(11) 0.0504(4) Uani 1 1 d . . . . .
 C23 C 0.31503(12) 0.24742(6) 0.86187(11) 0.0246(3) Uani 1 1 d . . . . .
 C55 C 0.21128(12) 0.28092(6) 0.41758(11) 0.0242(3) Uani 1 1 d . . . . .
 C42 C 0.55612(13) 0.30069(6) 0.59938(11) 0.0252(3) Uani 1 1 d . . . . .
 C65 C 0.41564(13) 0.12661(6) 0.47557(11) 0.0253(3) Uani 1 1 d . . . . .
 C7 C 0.12402(13) 0.39694(7) 0.69005(12) 0.0285(4) Uani 1 1 d . . . . .
 C49 C 0.23912(13) 0.27177(6) 0.28812(11) 0.0269(4) Uani 1 1 d . . . . .
 H49 H 0.208794 0.270786 0.229765 0.032 Uiso 1 1 calc R . . . .
 C50 C 0.17999(13) 0.28648(6) 0.33025(12) 0.0265(4) Uani 1 1 d . . . . .
 C70 C 0.38737(14) 0.11667(7) 0.39150(12) 0.0297(4) Uani 1 1 d . . . . .
 H70 H 0.376625 0.139467 0.352893 0.036 Uiso 1 1 calc R . . . .
 C37 C 0.57996(13) 0.31710(6) 0.68182(12) 0.0272(4) Uani 1 1 d . . . . .
 C20 C 0.46894(13) 0.42307(6) 0.87408(13) 0.0278(4) Uani 1 1 d . . . . .
 C22 C 0.31486(12) 0.29209(6) 0.82292(11) 0.0247(3) Uani 1 1 d . . . . .
 C57 C 0.37430(13) 0.36224(6) 0.46436(12) 0.0267(4) Uani 1 1 d . . . . .
 C45 C 0.46623(14) 0.26154(7) 0.27581(11) 0.0277(4) Uani 1 1 d . . . . .
 C24 C 0.34856(13) 0.24187(7) 0.94847(12) 0.0285(4) Uani 1 1 d . . . . .
 H24 H 0.370520 0.266261 0.983941 0.034 Uiso 1 1 calc R . . . .
 C43 C 0.60594(13) 0.29414(7) 0.48182(12) 0.0281(4) Uani 1 1 d . . . . .
 H43 H 0.656366 0.298844 0.465345 0.034 Uiso 1 1 calc R . . . .
 C30 C 0.16313(14) 0.51115(7) 0.77909(12) 0.0298(4) Uani 1 1 d . . . . .
 C14 C 0.44178(13) 0.41765(6) 1.00434(12) 0.0282(4) Uani 1 1 d . . . . .
 H14 H 0.468078 0.423820 1.061555 0.034 Uiso 1 1 calc R . . . .
 O8 O 0.31322(17) 0.48907(8) 0.7791(2) 0.0833(9) Uani 1 1 d . . . . .
 C54 C 0.14502(13) 0.29350(6) 0.45247(12) 0.0269(4) Uani 1 1 d . . . . .
 C8 C 0.07507(13) 0.37949(7) 0.80488(13) 0.0301(4) Uani 1 1 d . . . . .
 H8 H 0.022456 0.373427 0.817846 0.036 Uiso 1 1 calc R . . . .
 C10 C 0.22751(14) 0.37737(7) 1.02090(12) 0.0281(4) Uani 1 1 d . . . . .
 C64 C 0.42584(13) 0.17406(6) 0.50579(11) 0.0256(3) Uani 1 1 d . . . . .
 C6 C 0.05228(14) 0.39600(7) 0.72203(13) 0.0314(4) Uani 1 1 d . . . . .
 C9 C 0.16451(13) 0.35209(7) 0.94059(12) 0.0285(4) Uani 1 1 d . . . . .
 H9A H 0.189691 0.322146 0.944885 0.034 Uiso 1 1 calc R . . . .
 H9B H 0.098590 0.350022 0.936781 0.034 Uiso 1 1 calc R . . . .
 C44 C 0.54508(14) 0.24947(7) 0.36224(12) 0.0295(4) Uani 1 1 d . . . . .
 H44A H 0.544799 0.217570 0.369401 0.035 Uiso 1 1 calc R . . . .
 H44B H 0.608247 0.257582 0.364201 0.035 Uiso 1 1 calc R . . . .
 C48 C 0.36847(14) 0.24148(7) 0.26550(11) 0.0292(4) Uani 1 1 d . . . . .
 H48A H 0.321083 0.246173 0.208138 0.035 Uiso 1 1 calc R . . . .
 H48B H 0.376643 0.209724 0.274617 0.035 Uiso 1 1 calc R . . . .
 C41 C 0.61698(13) 0.31365(7) 0.56051(12) 0.0282(4) Uani 1 1 d . . . . .
 C38 C 0.65826(15) 0.34486(8) 0.72142(13) 0.0339(4) Uani 1 1 d . . . . .
 H38 H 0.672821 0.354854 0.775548 0.041 Uiso 1 1 calc R . . . .
 C31 C 0.08547(15) 0.50135(7) 0.79882(12) 0.0318(4) Uani 1 1 d . . . . .
 H31 H 0.087299 0.475919 0.829477 0.038 Uiso 1 1 calc R . . . .
 C51 C 0.08586(14) 0.30274(7) 0.27957(12) 0.0299(4) Uani 1 1 d . . . . .
 H51 H 0.066239 0.305958 0.222013 0.036 Uiso 1 1 calc R . . . .
 C13 C 0.33557(13) 0.37391(7) 1.03819(12) 0.0288(4) Uani 1 1 d . . . . .
 H13A H 0.373844 0.387724 1.091997 0.035 Uiso 1 1 calc R . . . .
 H13B H 0.353318 0.342775 1.043073 0.035 Uiso 1 1 calc R . . . .
 C58 C 0.33879(14) 0.40277(7) 0.40900(13) 0.0299(4) Uani 1 1 d . . . . .
 C53 C 0.05273(14) 0.30899(7) 0.40214(13) 0.0307(4) Uani 1 1 d . . . . .
 H53 H 0.009912 0.316268 0.425980 0.037 Uiso 1 1 calc R . . . .
 C2 C 0.09585(15) 0.41337(7) 0.60712(13) 0.0329(4) Uani 1 1 d . . . . .
 C15 C 0.49348(13) 0.43535(7) 0.95763(13) 0.0295(4) Uani 1 1 d . . . . .
 C28 C 0.28039(14) 0.21071(7) 0.80971(12) 0.0302(4) Uani 1 1 d . . . . .
 H28 H 0.257898 0.214083 0.751887 0.036 Uiso 1 1 calc R . . . .
 C25 C 0.34927(14) 0.20000(7) 0.98195(13) 0.0326(4) Uani 1 1 d . . . . .
 H25 H 0.373514 0.196394 1.039840 0.039 Uiso 1 1 calc R . . . .
 C66 C 0.43139(16) 0.09190(7) 0.53233(13) 0.0338(4) Uani 1 1 d . . . . .
 H66 H 0.450943 0.098092 0.589052 0.041 Uiso 1 1 calc R . . . .
 C11 C 0.19461(15) 0.42571(7) 1.01532(13) 0.0315(4) Uani 1 1 d . . . . .
 H11A H 0.202568 0.440091 0.969706 0.047 Uiso 1 1 calc GR . . . .
 H11B H 0.233448 0.440664 1.066938 0.047 Uiso 1 1 calc GR . . . .
 H11C H 0.127152 0.426731 1.005830 0.047 Uiso 1 1 calc GR . . . .
 C52 C 0.02303(14) 0.31385(7) 0.31519(13) 0.0324(4) Uani 1 1 d . . . . .
 H52 H -0.039026 0.324557 0.281746 0.039 Uiso 1 1 calc R . . . .
 C47 C 0.46001(15) 0.31156(7) 0.26312(13) 0.0332(4) Uani 1 1 d . . . . .
 H47A H 0.439104 0.325044 0.302470 0.050 Uiso 1 1 calc GR . . . .
 H47B H 0.413941 0.318293 0.206935 0.050 Uiso 1 1 calc GR . . . .
 H47C H 0.523046 0.322918 0.271957 0.050 Uiso 1 1 calc GR . . . .
 C26 C 0.31398(15) 0.16352(7) 0.92946(14) 0.0352(4) Uani 1 1 d . . . . .
 H26 H 0.313749 0.135603 0.951961 0.042 Uiso 1 1 calc R . . . .
 C68 C 0.39002(16) 0.03868(7) 0.42080(14) 0.0368(4) Uani 1 1 d . . . . .
 H68 H 0.381334 0.009413 0.402366 0.044 Uiso 1 1 calc R . . . .
 C29 C 0.24967(15) 0.48047(7) 0.80223(14) 0.0358(4) Uani 1 1 d . . . . .
 C36 C 0.54979(15) 0.31103(7) 0.80478(12) 0.0319(4) Uani 1 1 d . . . . .
 H36A H 0.507587 0.295651 0.824428 0.048 Uiso 1 1 calc GR . . . .
 H36B H 0.547338 0.342284 0.814205 0.048 Uiso 1 1 calc GR . . . .
 H36C H 0.615500 0.300581 0.834675 0.048 Uiso 1 1 calc GR . . . .
 C59 C 0.28913(15) 0.39872(7) 0.32227(14) 0.0346(4) Uani 1 1 d . . . . .
 H59 H 0.279772 0.370872 0.297265 0.042 Uiso 1 1 calc R . . . .
 C39 C 0.71642(15) 0.35818(8) 0.68020(14) 0.0388(5) Uani 1 1 d . . . . .
 H39 H 0.768204 0.377634 0.706459 0.047 Uiso 1 1 calc R . . . .
 C32 C 0.00517(15) 0.52909(8) 0.77329(14) 0.0381(5) Uani 1 1 d . . . . .
 H32 H -0.046703 0.522080 0.786679 0.046 Uiso 1 1 calc R . . . .
 C19 C 0.52859(15) 0.43999(7) 0.83508(15) 0.0342(4) Uani 1 1 d . . . . .
 C12 C 0.21380(16) 0.35374(8) 1.09270(13) 0.0368(4) Uani 1 1 d . . . . .
 H12A H 0.147795 0.357611 1.086118 0.055 Uiso 1 1 calc GR . . . .
 H12B H 0.257824 0.366124 1.145439 0.055 Uiso 1 1 calc GR . . . .
 H12C H 0.227213 0.322678 1.091497 0.055 Uiso 1 1 calc GR . . . .
 C16 C 0.57579(15) 0.46230(7) 1.00201(16) 0.0375(4) Uani 1 1 d . . . . .
 H16 H 0.591975 0.469500 1.057855 0.045 Uiso 1 1 calc R . . . .
 C67 C 0.41812(17) 0.04815(7) 0.50492(14) 0.0381(5) Uani 1 1 d . . . . .
 H67 H 0.428145 0.025227 0.543159 0.046 Uiso 1 1 calc R . . . .
 C56 C 0.11584(15) 0.29845(8) 0.57598(13) 0.0360(4) Uani 1 1 d . . . . .
 H56A H 0.061503 0.278347 0.555288 0.054 Uiso 1 1 calc GR . . . .
 H56B H 0.092629 0.328321 0.562086 0.054 Uiso 1 1 calc GR . . . .
 H56C H 0.149526 0.295535 0.635859 0.054 Uiso 1 1 calc GR . . . .
 C69 C 0.37494(18) 0.07280(8) 0.36439(14) 0.0387(5) Uani 1 1 d . . . . .
 H69 H 0.356342 0.066458 0.307843 0.046 Uiso 1 1 calc R . . . .
 C40 C 0.69676(14) 0.34252(8) 0.60160(13) 0.0355(4) Uani 1 1 d . . . . .
 H40 H 0.736092 0.350906 0.574964 0.043 Uiso 1 1 calc R . . . .
 C27 C 0.27906(16) 0.16906(7) 0.84314(14) 0.0357(4) Uani 1 1 d . . . . .
 H27 H 0.254722 0.144833 0.807607 0.043 Uiso 1 1 calc R . . . .
 C46 C 0.49469(16) 0.23942(8) 0.21023(13) 0.0372(5) Uani 1 1 d . . . . .
 H46A H 0.558142 0.249584 0.217702 0.056 Uiso 1 1 calc GR . . . .
 H46B H 0.447736 0.247064 0.154865 0.056 Uiso 1 1 calc GR . . . .
 H46C H 0.495966 0.207808 0.217153 0.056 Uiso 1 1 calc GR . . . .
 C73 C 0.18276(17) 0.14848(9) 0.49843(14) 0.0404(5) Uani 1 1 d . . . . .
 H73A H 0.159662 0.122768 0.462169 0.049 Uiso 1 1 calc R . . . .
 H73B H 0.220446 0.167119 0.477815 0.049 Uiso 1 1 calc R . . . .
 C5 C -0.04333(15) 0.41075(9) 0.67179(14) 0.0401(5) Uani 1 1 d . . . . .
 H5 H -0.090386 0.409300 0.693042 0.048 Uiso 1 1 calc R . . . .
 C72 C 0.09675(17) 0.17446(8) 0.50241(14) 0.0385(5) Uani 1 1 d . . . . .
 H72A H 0.094107 0.204507 0.481753 0.046 Uiso 1 1 calc R . . . .
 H72B H 0.035055 0.159806 0.470111 0.046 Uiso 1 1 calc R . . . .
 C35 C 0.15966(16) 0.54964(8) 0.73414(15) 0.0395(5) Uani 1 1 d . . . . .
 H35 H 0.211689 0.556725 0.721005 0.047 Uiso 1 1 calc R . . . .
 C17 C 0.63169(16) 0.47782(8) 0.96331(18) 0.0448(5) Uani 1 1 d . . . . .
 H17 H 0.685636 0.495627 0.992668 0.054 Uiso 1 1 calc R . . . .
 C18 C 0.60755(17) 0.46683(8) 0.87930(18) 0.0435(5) Uani 1 1 d . . . . .
 H18 H 0.645284 0.477782 0.852981 0.052 Uiso 1 1 calc R . . . .
 C33 C 0.00139(16) 0.56717(8) 0.72803(14) 0.0400(5) Uani 1 1 d . . . . .
 H33 H -0.052887 0.585658 0.710681 0.048 Uiso 1 1 calc R . . . .
 C74 C 0.24360(18) 0.13452(8) 0.58915(14) 0.0434(5) Uani 1 1 d . . . . .
 H74A H 0.223543 0.105576 0.600359 0.052 Uiso 1 1 calc R . . . .
 H74B H 0.312449 0.133504 0.601074 0.052 Uiso 1 1 calc R . . . .
 C63 C 0.35218(19) 0.44493(8) 0.44475(17) 0.0434(5) Uani 1 1 d . . . . .
 H63 H 0.384237 0.447957 0.502761 0.052 Uiso 1 1 calc R . . . .
 C34 C 0.07932(18) 0.57752(8) 0.70877(16) 0.0426(5) Uani 1 1 d . . . . .
 H34 H 0.077675 0.603191 0.678786 0.051 Uiso 1 1 calc R . . . .
 C3 C 0.00188(16) 0.42851(8) 0.56018(14) 0.0410(5) Uani 1 1 d . . . . .
 H3 H -0.014695 0.439717 0.506506 0.049 Uiso 1 1 calc R . . . .
 C4 C -0.06852(16) 0.42705(9) 0.59301(15) 0.0450(5) Uani 1 1 d . . . . .
 H4 H -0.131658 0.437099 0.561312 0.054 Uiso 1 1 calc R . . . .
 C61 C 0.26905(19) 0.47799(9) 0.3094(2) 0.0512(6) Uani 1 1 d . . . . .
 H61 H 0.246089 0.503040 0.275959 0.061 Uiso 1 1 calc R . . . .
 C60 C 0.25351(18) 0.43631(9) 0.27303(16) 0.0459(5) Uani 1 1 d . . . . .
 H60 H 0.218967 0.433448 0.215194 0.055 Uiso 1 1 calc R . . . .
 C62 C 0.3185(2) 0.48239(9) 0.3952(2) 0.0546(7) Uani 1 1 d . . . . .
 H62 H 0.329239 0.510370 0.419785 0.065 Uiso 1 1 calc R . . . .
 C71 C 0.1206(2) 0.17413(10) 0.59616(16) 0.0500(6) Uani 1 1 d . . . . .
 H71A H 0.101961 0.201986 0.613000 0.060 Uiso 1 1 calc R . . . .
 H71B H 0.086581 0.150146 0.609498 0.060 Uiso 1 1 calc R . . . .
 C21 C 0.5528(2) 0.44444(9) 0.7088(2) 0.0549(7) Uani 1 1 d . . . . .
 H21A H 0.529095 0.431381 0.653891 0.082 Uiso 1 1 calc GR . . . .
 H21B H 0.621181 0.438175 0.738807 0.082 Uiso 1 1 calc GR . . . .
 H21C H 0.543070 0.475956 0.703665 0.082 Uiso 1 1 calc GR . . . .
 C1 C 0.1443(2) 0.42698(12) 0.49599(16) 0.0569(7) Uani 1 1 d . . . . .
 H1A H 0.199440 0.422764 0.482768 0.085 Uiso 1 1 calc GR . . . .
 H1B H 0.127278 0.457855 0.491121 0.085 Uiso 1 1 calc GR . . . .
 H1C H 0.089961 0.410095 0.457687 0.085 Uiso 1 1 calc GR . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 K2 K1 3.7986(6) . ?
 K2 Al2 3.6286(6) . ?
 K2 O10 2.7330(12) . ?
 K2 O11 2.7296(13) . ?
 K2 O9 2.7923(15) . ?
 K2 O6 2.8076(14) . ?
 K2 O12 2.8129(14) . ?
 K2 O16 2.6571(15) . ?
 K2 O17 3.146(2) . ?
 K1 Al1 3.5995(6) . ?
 K1 O9 3.1304(15) . ?
 K1 O3 2.7137(14) . ?
 K1 O2 2.6588(13) . ?
 K1 O6 2.8365(15) . ?
 K1 O14 2.6320(14) . ?
 K1 O1 2.7808(16) . ?
 K1 O4 2.7698(18) . ?
 Al2 O10 1.8399(13) . ?
 Al2 O11 1.8432(12) . ?
 Al2 O13 1.9152(14) . ?
 Al2 O15 1.8982(14) . ?
 Al2 N3 2.0383(15) . ?
 Al2 N4 2.0743(16) . ?
 Al1 O7 1.8784(14) . ?
 Al1 O3 1.8364(12) . ?
 Al1 O2 1.8519(14) . ?
 Al1 O5 1.9060(15) . ?
 Al1 N1 2.0646(15) . ?
 Al1 N2 2.0584(16) . ?
 O10 C42 1.301(2) . ?
 O11 C55 1.313(2) . ?
 O13 C57 1.287(2) . ?
 O15 C64 1.288(2) . ?
 O7 C29 1.288(3) . ?
 O9 C37 1.377(2) . ?
 O9 C36 1.432(2) . ?
 O3 C20 1.306(2) . ?
 O2 C7 1.308(2) . ?
 O5 C22 1.275(2) . ?
 O6 C22 1.240(2) . ?
 O12 C54 1.379(2) . ?
 O12 C56 1.427(2) . ?
 O16 C64 1.233(2) . ?
 O14 C57 1.229(2) . ?
 O1 C2 1.369(3) . ?
 O1 C1 1.422(3) . ?
 O4 C19 1.375(3) . ?
 O4 C21 1.426(2) . ?
 N3 C43 1.283(3) . ?
 N3 C44 1.464(2) . ?
 N1 C8 1.286(3) . ?
 N1 C9 1.465(2) . ?
 N4 C49 1.286(3) . ?
 N4 C48 1.469(2) . ?
 N2 C14 1.290(3) . ?
 N2 C13 1.470(2) . ?
 O17 C74 1.420(3) . ?
 O17 C71 1.443(3) . ?
 C23 C22 1.509(3) . ?
 C23 C24 1.395(3) . ?
 C23 C28 1.391(3) . ?
 C55 C50 1.411(2) . ?
 C55 C54 1.423(2) . ?
 C42 C37 1.424(3) . ?
 C42 C41 1.407(3) . ?
 C65 C70 1.385(3) . ?
 C65 C64 1.511(3) . ?
 C65 C66 1.394(3) . ?
 C7 C6 1.411(3) . ?
 C7 C2 1.422(3) . ?
 C49 C50 1.445(3) . ?
 C50 C51 1.411(3) . ?
 C70 C69 1.391(3) . ?
 C37 C38 1.375(3) . ?
 C20 C15 1.402(3) . ?
 C20 C19 1.432(3) . ?
 C57 C58 1.512(3) . ?
 C45 C44 1.528(3) . ?
 C45 C48 1.533(3) . ?
 C45 C47 1.522(3) . ?
 C45 C46 1.537(2) . ?
 C24 C25 1.390(3) . ?
 C43 C41 1.444(3) . ?
 C30 C31 1.384(3) . ?
 C30 C29 1.510(3) . ?
 C30 C35 1.391(3) . ?
 C14 C15 1.448(3) . ?
 O8 C29 1.214(3) . ?
 C54 C53 1.381(3) . ?
 C8 C6 1.434(3) . ?
 C10 C9 1.532(3) . ?
 C10 C13 1.531(3) . ?
 C10 C11 1.530(3) . ?
 C10 C12 1.533(3) . ?
 C6 C5 1.411(3) . ?
 C41 C40 1.414(3) . ?
 C38 C39 1.408(3) . ?
 C31 C32 1.383(3) . ?
 C51 C52 1.376(3) . ?
 C58 C59 1.391(3) . ?
 C58 C63 1.394(3) . ?
 C53 C52 1.405(3) . ?
 C2 C3 1.385(3) . ?
 C15 C16 1.414(3) . ?
 C28 C27 1.389(3) . ?
 C25 C26 1.389(3) . ?
 C66 C67 1.389(3) . ?
 C26 C27 1.389(3) . ?
 C68 C67 1.383(3) . ?
 C68 C69 1.378(3) . ?
 C59 C60 1.389(3) . ?
 C39 C40 1.366(3) . ?
 C32 C33 1.383(3) . ?
 C19 C18 1.379(3) . ?
 C16 C17 1.367(3) . ?
 C73 C72 1.541(3) . ?
 C73 C74 1.526(3) . ?
 C5 C4 1.361(3) . ?
 C72 C71 1.528(3) . ?
 C35 C34 1.386(3) . ?
 C17 C18 1.401(4) . ?
 C33 C34 1.387(3) . ?
 C63 C62 1.385(4) . ?
 C3 C4 1.404(3) . ?
 C61 C60 1.384(4) . ?
 C61 C62 1.377(5) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 Al2 K2 K1 92.034(14) . . ?
 O10 K2 K1 83.08(3) . . ?
 O10 K2 Al2 29.57(3) . . ?
 O10 K2 O9 57.08(4) . . ?
 O10 K2 O6 125.78(4) . . ?
 O10 K2 O12 104.95(4) . . ?
 O10 K2 O17 143.17(4) . . ?
 O11 K2 K1 88.79(3) . . ?
 O11 K2 Al2 29.62(3) . . ?
 O11 K2 O10 57.78(4) . . ?
 O11 K2 O9 106.68(4) . . ?
 O11 K2 O6 128.02(4) . . ?
 O11 K2 O12 56.73(4) . . ?
 O11 K2 O17 102.63(4) . . ?
 O9 K2 K1 54.14(3) . . ?
 O9 K2 Al2 84.92(3) . . ?
 O9 K2 O6 73.53(4) . . ?
 O9 K2 O12 115.85(5) . . ?
 O9 K2 O17 150.51(4) . . ?
 O6 K2 K1 48.02(3) . . ?
 O6 K2 Al2 139.99(3) . . ?
 O6 K2 O12 76.05(4) . . ?
 O6 K2 O17 91.03(4) . . ?
 O12 K2 K1 63.38(3) . . ?
 O12 K2 Al2 84.09(3) . . ?
 O12 K2 O17 83.17(5) . . ?
 O16 K2 K1 148.65(3) . . ?
 O16 K2 Al2 61.25(3) . . ?
 O16 K2 O10 65.59(4) . . ?
 O16 K2 O11 75.69(4) . . ?
 O16 K2 O9 104.05(5) . . ?
 O16 K2 O6 156.19(5) . . ?
 O16 K2 O12 123.97(5) . . ?
 O16 K2 O17 79.95(5) . . ?
 O17 K2 K1 130.62(4) . . ?
 O17 K2 Al2 120.95(3) . . ?
 Al1 K1 K2 109.739(15) . . ?
 O9 K1 K2 46.30(3) . . ?
 O9 K1 Al1 110.58(3) . . ?
 O3 K1 K2 116.58(3) . . ?
 O3 K1 Al1 29.83(3) . . ?
 O3 K1 O9 94.03(4) . . ?
 O3 K1 O6 75.23(4) . . ?
 O3 K1 O1 104.83(4) . . ?
 O3 K1 O4 57.45(4) . . ?
 O2 K1 K2 108.18(3) . . ?
 O2 K1 Al1 29.88(3) . . ?
 O2 K1 O9 132.19(4) . . ?
 O2 K1 O3 58.54(4) . . ?
 O2 K1 O6 67.27(4) . . ?
 O2 K1 O1 57.90(4) . . ?
 O2 K1 O4 108.52(5) . . ?
 O6 K1 K2 47.38(3) . . ?
 O6 K1 Al1 62.36(3) . . ?
 O6 K1 O9 68.14(4) . . ?
 O14 K1 K2 74.66(4) . . ?
 O14 K1 Al1 175.16(4) . . ?
 O14 K1 O9 73.83(4) . . ?
 O14 K1 O3 150.28(5) . . ?
 O14 K1 O2 147.65(5) . . ?
 O14 K1 O6 122.00(5) . . ?
 O14 K1 O1 91.64(5) . . ?
 O14 K1 O4 93.31(5) . . ?
 O1 K1 K2 117.76(4) . . ?
 O1 K1 Al1 84.52(3) . . ?
 O1 K1 O9 160.36(5) . . ?
 O1 K1 O6 111.08(5) . . ?
 O4 K1 K2 126.29(4) . . ?
 O4 K1 Al1 85.64(3) . . ?
 O4 K1 O9 79.99(4) . . ?
 O4 K1 O6 120.08(5) . . ?
 O4 K1 O1 114.68(5) . . ?
 O10 Al2 K2 47.14(4) . . ?
 O10 Al2 O11 91.55(6) . . ?
 O10 Al2 O13 94.30(6) . . ?
 O10 Al2 O15 95.96(6) . . ?
 O10 Al2 N3 89.27(6) . . ?
 O10 Al2 N4 177.73(7) . . ?
 O11 Al2 K2 47.05(4) . . ?
 O11 Al2 O13 91.89(6) . . ?
 O11 Al2 O15 93.19(6) . . ?
 O11 Al2 N3 178.48(7) . . ?
 O11 Al2 N4 90.03(6) . . ?
 O13 Al2 K2 107.00(4) . . ?
 O13 Al2 N3 86.77(6) . . ?
 O13 Al2 N4 84.02(6) . . ?
 O15 Al2 K2 84.00(4) . . ?
 O15 Al2 O13 168.42(6) . . ?
 O15 Al2 N3 87.99(6) . . ?
 O15 Al2 N4 85.58(6) . . ?
 N3 Al2 K2 134.10(5) . . ?
 N3 Al2 N4 89.11(6) . . ?
 N4 Al2 K2 134.85(4) . . ?
 O7 Al1 K1 108.17(4) . . ?
 O7 Al1 O5 166.72(6) . . ?
 O7 Al1 N1 85.65(6) . . ?
 O7 Al1 N2 86.35(6) . . ?
 O3 Al1 K1 47.30(4) . . ?
 O3 Al1 O7 98.24(6) . . ?
 O3 Al1 O2 90.85(6) . . ?
 O3 Al1 O5 92.46(6) . . ?
 O3 Al1 N1 176.07(7) . . ?
 O3 Al1 N2 90.18(6) . . ?
 O2 Al1 K1 45.66(4) . . ?
 O2 Al1 O7 91.75(6) . . ?
 O2 Al1 O5 95.97(6) . . ?
 O2 Al1 N1 88.45(6) . . ?
 O2 Al1 N2 177.95(7) . . ?
 O5 Al1 K1 84.89(4) . . ?
 O5 Al1 N1 83.77(6) . . ?
 O5 Al1 N2 85.76(6) . . ?
 N1 Al1 K1 130.90(5) . . ?
 N2 Al1 K1 135.79(4) . . ?
 N2 Al1 N1 90.64(6) . . ?
 Al2 O10 K2 103.29(5) . . ?
 C42 O10 K2 125.56(11) . . ?
 C42 O10 Al2 126.28(11) . . ?
 Al2 O11 K2 103.32(5) . . ?
 C55 O11 K2 126.36(10) . . ?
 C55 O11 Al2 126.09(11) . . ?
 C57 O13 Al2 134.82(12) . . ?
 C64 O15 Al2 131.41(12) . . ?
 C29 O7 Al1 133.12(13) . . ?
 K2 O9 K1 79.56(4) . . ?
 C37 O9 K2 123.23(11) . . ?
 C37 O9 K1 109.29(11) . . ?
 C37 O9 C36 116.45(15) . . ?
 C36 O9 K2 119.18(11) . . ?
 C36 O9 K1 91.90(10) . . ?
 Al1 O3 K1 102.87(6) . . ?
 C20 O3 K1 125.65(11) . . ?
 C20 O3 Al1 127.07(12) . . ?
 Al1 O2 K1 104.46(6) . . ?
 C7 O2 K1 125.61(11) . . ?
 C7 O2 Al1 126.06(12) . . ?
 C22 O5 Al1 135.47(12) . . ?
 K2 O6 K1 84.60(4) . . ?
 C22 O6 K2 145.44(13) . . ?
 C22 O6 K1 127.31(13) . . ?
 C54 O12 K2 123.08(10) . . ?
 C54 O12 C56 116.52(15) . . ?
 C56 O12 K2 119.63(12) . . ?
 C64 O16 K2 128.92(13) . . ?
 C57 O14 K1 163.76(14) . . ?
 C2 O1 K1 121.41(12) . . ?
 C2 O1 C1 117.36(18) . . ?
 C1 O1 K1 120.30(14) . . ?
 C19 O4 K1 123.43(11) . . ?
 C19 O4 C21 117.3(2) . . ?
 C21 O4 K1 119.16(17) . . ?
 C43 N3 Al2 120.67(12) . . ?
 C43 N3 C44 116.03(15) . . ?
 C44 N3 Al2 123.28(12) . . ?
 C8 N1 Al1 121.61(13) . . ?
 C8 N1 C9 116.42(15) . . ?
 C9 N1 Al1 121.96(12) . . ?
 C49 N4 Al2 120.41(12) . . ?
 C49 N4 C48 115.49(16) . . ?
 C48 N4 Al2 124.09(12) . . ?
 C14 N2 Al1 120.20(13) . . ?
 C14 N2 C13 115.32(16) . . ?
 C13 N2 Al1 124.48(12) . . ?
 C74 O17 K2 103.16(14) . . ?
 C74 O17 C71 103.72(19) . . ?
 C71 O17 K2 117.93(16) . . ?
 C24 C23 C22 122.04(17) . . ?
 C28 C23 C22 118.91(17) . . ?
 C28 C23 C24 119.05(18) . . ?
 O11 C55 C50 123.55(16) . . ?
 O11 C55 C54 119.15(16) . . ?
 C50 C55 C54 117.24(17) . . ?
 O10 C42 C37 119.71(16) . . ?
 O10 C42 C41 123.16(17) . . ?
 C41 C42 C37 117.08(17) . . ?
 C70 C65 C64 121.27(17) . . ?
 C70 C65 C66 118.79(18) . . ?
 C66 C65 C64 119.90(17) . . ?
 O2 C7 C6 122.89(18) . . ?
 O2 C7 C2 119.58(17) . . ?
 C6 C7 C2 117.49(18) . . ?
 N4 C49 C50 126.91(17) . . ?
 C55 C50 C49 121.33(17) . . ?
 C55 C50 C51 121.12(17) . . ?
 C51 C50 C49 117.28(17) . . ?
 C65 C70 C69 120.45(19) . . ?
 O9 C37 C42 114.38(16) . . ?
 C38 C37 O9 124.09(17) . . ?
 C38 C37 C42 121.53(17) . . ?
 O3 C20 C15 123.45(16) . . ?
 O3 C20 C19 119.11(19) . . ?
 C15 C20 C19 117.40(19) . . ?
 O5 C22 C23 114.67(15) . . ?
 O6 C22 O5 126.29(18) . . ?
 O6 C22 C23 119.04(16) . . ?
 O13 C57 C58 114.44(15) . . ?
 O14 C57 O13 126.69(18) . . ?
 O14 C57 C58 118.87(17) . . ?
 C44 C45 C48 109.54(15) . . ?
 C44 C45 C46 107.06(16) . . ?
 C48 C45 C46 107.22(16) . . ?
 C47 C45 C44 110.84(17) . . ?
 C47 C45 C48 112.10(16) . . ?
 C47 C45 C46 109.89(16) . . ?
 C25 C24 C23 120.24(19) . . ?
 N3 C43 C41 126.32(16) . . ?
 C31 C30 C29 121.90(18) . . ?
 C31 C30 C35 118.93(19) . . ?
 C35 C30 C29 119.13(18) . . ?
 N2 C14 C15 126.76(18) . . ?
 O12 C54 C55 114.30(16) . . ?
 O12 C54 C53 124.59(16) . . ?
 C53 C54 C55 121.10(17) . . ?
 N1 C8 C6 126.83(17) . . ?
 C9 C10 C12 106.17(16) . . ?
 C13 C10 C9 110.36(15) . . ?
 C13 C10 C12 107.65(16) . . ?
 C11 C10 C9 110.81(16) . . ?
 C11 C10 C13 111.55(16) . . ?
 C11 C10 C12 110.11(16) . . ?
 O15 C64 C65 115.49(15) . . ?
 O16 C64 O15 126.28(18) . . ?
 O16 C64 C65 118.22(17) . . ?
 C7 C6 C8 120.65(18) . . ?
 C5 C6 C7 119.92(19) . . ?
 C5 C6 C8 119.42(18) . . ?
 N1 C9 C10 114.53(16) . . ?
 N3 C44 C45 114.20(15) . . ?
 N4 C48 C45 114.32(15) . . ?
 C42 C41 C43 120.73(18) . . ?
 C42 C41 C40 120.83(18) . . ?
 C40 C41 C43 118.12(16) . . ?
 C37 C38 C39 120.16(19) . . ?
 C32 C31 C30 120.5(2) . . ?
 C52 C51 C50 120.08(18) . . ?
 N2 C13 C10 115.74(16) . . ?
 C59 C58 C57 120.98(18) . . ?
 C59 C58 C63 118.8(2) . . ?
 C63 C58 C57 120.16(19) . . ?
 C54 C53 C52 120.49(17) . . ?
 O1 C2 C7 114.37(18) . . ?
 O1 C2 C3 124.54(19) . . ?
 C3 C2 C7 121.09(19) . . ?
 C20 C15 C14 121.58(18) . . ?
 C20 C15 C16 120.96(18) . . ?
 C16 C15 C14 117.20(19) . . ?
 C27 C28 C23 120.64(18) . . ?
 C26 C25 C24 120.41(18) . . ?
 C67 C66 C65 120.59(19) . . ?
 C51 C52 C53 119.93(18) . . ?
 C27 C26 C25 119.5(2) . . ?
 C69 C68 C67 119.7(2) . . ?
 O7 C29 C30 114.96(16) . . ?
 O8 C29 O7 125.5(2) . . ?
 O8 C29 C30 119.6(2) . . ?
 C60 C59 C58 119.9(2) . . ?
 C40 C39 C38 120.0(2) . . ?
 C31 C32 C33 120.55(19) . . ?
 O4 C19 C20 114.33(19) . . ?
 O4 C19 C18 125.14(19) . . ?
 C18 C19 C20 120.5(2) . . ?
 C17 C16 C15 120.4(2) . . ?
 C68 C67 C66 120.0(2) . . ?
 C68 C69 C70 120.4(2) . . ?
 C39 C40 C41 120.41(18) . . ?
 C26 C27 C28 120.2(2) . . ?
 C74 C73 C72 104.13(18) . . ?
 C4 C5 C6 121.73(19) . . ?
 C71 C72 C73 102.75(19) . . ?
 C34 C35 C30 120.6(2) . . ?
 C16 C17 C18 119.8(2) . . ?
 C19 C18 C17 120.9(2) . . ?
 C32 C33 C34 119.4(2) . . ?
 O17 C74 C73 104.3(2) . . ?
 C62 C63 C58 121.0(2) . . ?
 C35 C34 C33 120.1(2) . . ?
 C2 C3 C4 120.5(2) . . ?
 C5 C4 C3 119.3(2) . . ?
 C62 C61 C60 120.0(2) . . ?
 C61 C60 C59 120.5(2) . . ?
 C61 C62 C63 119.7(3) . . ?
 O17 C71 C72 105.24(19) . . ?

_smtbx_masks_special_details       ?
loop_
  _smtbx_masks_void_nr
  _smtbx_masks_void_average_x
  _smtbx_masks_void_average_y
  _smtbx_masks_void_average_z
  _smtbx_masks_void_volume
  _smtbx_masks_void_count_electrons
  _smtbx_masks_void_content
 1 -0.103 -0.062 0.144 163.2 41.2 THF
 2 0.103 0.062 0.856 163.2 39.6 THF
 3 0.397 0.562 0.644 163.2 40.0 THF
 4 0.603 0.438 0.356 163.2 40.8 THF


_ins_header
;
TITL 021RWFK21 in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  15.077907  30.147922  17.524862  90.0000 114.6993  90.0000
ZERR    7.00   0.000209   0.000395   0.000256   0.0000   0.0018   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H N O Al K
UNIT 700.00 700.00 28.00 70.00 7.00 7.00
TREF
HKLF 4
END
;
_olex2_date_sample_data_collection  2021-06-04
_olex2_submission_special_instructions  'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max  1.395
_oxdiff_exptl_absorpt_empirical_full_min  0.633
