# [Zn4(C6H12N2)(C3H6O3)2(C6H2SO4)2]*DMF*4H2O
data_al65_sq

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H43 N3 O19 S2 Zn4'
_chemical_formula_weight         1039.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0070 0.0030 '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'
N N 0.0130 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0210 0.0120 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1970 0.2290 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -0.2060 2.4400 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_H-M_alt        'R -3 m :H'
_space_group_name_Hall           '-R 3 2"'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   32.0133(5)
_cell_length_b                   32.0133(5)
_cell_length_c                   11.7265(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     10407.8(4)
_cell_formula_units_Z            9
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    600
_cell_measurement_theta_min      3.5
_cell_measurement_theta_max      30.0

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_F_000             4770
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    5.031
_shelx_estimated_absorpt_T_min   0.633
_shelx_estimated_absorpt_T_max   0.787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_T_max  0.780
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_absorpt_special_details   ?

_diffrn_radiation_source         synchrotron
_diffrn_radiation_monochromator  'Double Crystal Monochromator'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.80246
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'Rayonix SX-165 CCD'
_diffrn_measurement_method       'φ scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28847
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_av_R_equivalents  0.0748
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.474
_diffrn_reflns_theta_max         36.254
_diffrn_reflns_theta_full        35.587
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2333
_reflns_number_gt                1613
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;
_computing_data_collection       'Marccd (Doyle, 2011)'
_computing_cell_refinement       'iMosflm (Battye et al., 2011)'
_computing_data_reduction        iMosflm
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1061P)²+15.4000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00015(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2333
_refine_ls_number_parameters     159
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0604
_refine_ls_wR_factor_ref         0.2050
_refine_ls_wR_factor_gt          0.1876
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.146
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
Zn1 Zn 0.78723(2) 0.57447(3) 0.86091(7) 0.0805(4) Uani 1 2 d S T P . .
Zn2 Zn 0.666667 0.52946(4) 0.833333 0.1153(5) Uani 1 2 d S T P . .
O11 O 0.65304(16) 0.56467(17) 0.7122(4) 0.1245(16) Uani 1 1 d . . . . .
O12 O 0.57526(14) 0.50969(16) 0.6901(3) 0.1050(13) Uani 1 1 d . . . . .
C11 C 0.6131(2) 0.5490(2) 0.6678(4) 0.0907(15) Uani 1 1 d . . . . .
C12 C 0.60927(17) 0.57959(19) 0.5767(4) 0.0845(15) Uani 1 1 d . . . . .
C13 C 0.6416(2) 0.6240(2) 0.5427(4) 0.1013(18) Uani 1 1 d . . . . .
H13 H 0.673290 0.641714 0.573220 0.122 Uiso 1 1 calc R U . . .
S1 S 0.55647(5) 0.55647(5) 0.500000 0.0863(6) Uani 1 2 d S T P . .
N1 N 0.81584(10) 0.6317(2) 0.7422(4) 0.0748(13) Uani 1 2 d DS TU P . .
C1 C 0.7817(3) 0.6482(3) 0.7155(7) 0.095(3) Uani 0.5 1 d D U P . .
H1A H 0.776599 0.663109 0.784280 0.114 Uiso 0.5 1 calc R U P . .
H1B H 0.750217 0.620204 0.693830 0.114 Uiso 0.5 1 calc R U P . .
C2 C 0.8613(3) 0.6743(3) 0.7847(8) 0.114(4) Uani 0.5 1 d D U P . .
H2A H 0.886652 0.665417 0.793542 0.137 Uiso 0.5 1 calc R U P . .
H2B H 0.855454 0.684187 0.860279 0.137 Uiso 0.5 1 calc R U P . .
C3 C 0.8286(4) 0.6168(3) 0.6331(7) 0.094(3) Uani 0.5 1 d D U P . .
H3A H 0.798855 0.590791 0.597578 0.113 Uiso 0.5 1 calc R U P . .
H3B H 0.850184 0.603738 0.649534 0.113 Uiso 0.5 1 calc R U P . .
O22 O 0.72315(15) 0.52719(17) 0.7961(4) 0.1225(15) Uani 1 1 d D . . . .
O21 O 0.6506(9) 0.4757(9) 0.645(2) 0.196(7) Uani 0.25 1 d D U P A -1
O23 O 0.8037(9) 0.4454(9) 0.665(3) 0.195(7) Uani 0.25 1 d D U P A -1
H23A H 0.819483 0.449958 0.724916 0.292 Uiso 0.25 1 calc R U P A -1
C21 C 0.6897(10) 0.4683(11) 0.6444(17) 0.171(6) Uani 0.25 1 d D U P A -1
H21A H 0.711209 0.486635 0.580126 0.206 Uiso 0.25 1 calc R U P A -1
H21B H 0.678113 0.433690 0.631254 0.206 Uiso 0.25 1 calc R U P A -1
C22 C 0.7188(7) 0.4841(4) 0.7558(13) 0.166(5) Uani 0.5 1 d D U P A -1
C23 C 0.7699(6) 0.4970(4) 0.7173(13) 0.164(5) Uani 0.5 1 d D U P A -1
C24 C 0.7623(9) 0.4471(7) 0.688(3) 0.172(6) Uani 0.25 1 d D U P A -1
H24A H 0.745405 0.425091 0.752299 0.207 Uiso 0.25 1 calc R U P A -1
H24B H 0.740752 0.434657 0.620564 0.207 Uiso 0.25 1 calc R U P A -1


_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
Zn1 O12 2.057(4) 18_656 yes
Zn1 O12 2.058(4) 32_556 ?
Zn1 N1 2.110(6) . yes
Zn1 O22 1.993(4) . yes
Zn1 O22 1.993(4) 23_655 ?
Zn2 O11 1.993(5) . yes
Zn2 O11 1.993(5) 18_656 ?
Zn2 O22 1.897(5) . yes
Zn2 O22 1.897(5) 18_656 ?
O11 C11 1.231(7) . ?
O12 C11 1.263(7) . ?
C11 C12 1.494(8) . ?
C12 C13 1.333(8) . ?
C12 S1 1.722(5) . ?
C13 C13 1.401(12) 4_556 ?
C13 H13 0.9500 . ?
N1 C1 1.468(7) . ?
N1 C1 1.468(7) 23_655 ?
N1 C2 1.498(8) . ?
N1 C2 1.498(8) 23_655 ?
N1 C3 1.491(8) . ?
N1 C3 1.491(8) 23_655 ?
C1 C1 1.535(14) 11_566 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C3 2.031(15) 25_666 ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.539(13) 11_566 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
O22 C22 1.399(10) . ?
O22 C23 1.388(10) 23_655 ?
O21 C21 1.387(12) . ?
O23 H23A 0.8400 . ?
O23 C24 1.380(12) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.536(14) . ?
C22 C23 1.539(13) . ?
C23 C24 1.531(14) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?

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
O12 Zn1 O12 82.7(2) 18_656 32_556 ?
O12 Zn1 N1 99.50(16) 18_656 . ?
O12 Zn1 N1 99.50(17) 32_556 . ?
O22 Zn1 O12 93.32(16) 23_655 32_556 ?
O22 Zn1 O12 93.33(16) . 18_656 ?
O22 Zn1 O12 156.5(2) . 32_556 ?
O22 Zn1 O12 156.5(2) 23_655 18_656 ?
O22 Zn1 N1 104.04(18) . . ?
O22 Zn1 N1 104.04(18) 23_655 . ?
O22 Zn1 O22 81.0(3) 23_655 . ?
O11 Zn2 O11 95.1(3) 18_656 . ?
O22 Zn2 O11 109.9(2) . . ?
O22 Zn2 O11 109.9(2) 18_656 18_656 ?
O22 Zn2 O11 110.82(18) . 18_656 ?
O22 Zn2 O11 110.82(18) 18_656 . ?
O22 Zn2 O22 118.0(3) . 18_656 ?
C11 O11 Zn2 123.2(4) . . ?
C11 O12 Zn1 142.6(4) . 33_546 ?
O11 C11 O12 126.9(6) . . ?
O11 C11 C12 116.4(5) . . ?
O12 C11 C12 116.7(5) . . ?
C11 C12 S1 118.4(4) . . ?
C13 C12 C11 129.6(5) . . ?
C13 C12 S1 112.0(5) . . ?
C12 C13 C13 112.9(4) . 4_556 ?
C12 C13 H13 123.6 . . ?
C13 C13 H13 123.6 4_556 . ?
C12 S1 C12 90.2(4) 4_556 . ?
C1 N1 Zn1 112.1(3) . . ?
C1 N1 Zn1 112.1(3) 23_655 . ?
C1 N1 C1 135.5(7) 23_655 . ?
C1 N1 C2 49.2(6) . 23_655 ?
C1 N1 C2 49.2(6) 23_655 . ?
C1 N1 C2 107.6(6) . . ?
C1 N1 C2 107.6(6) 23_655 23_655 ?
C1 N1 C3 60.2(6) . 23_655 ?
C1 N1 C3 60.2(6) 23_655 . ?
C1 N1 C3 107.7(5) . . ?
C1 N1 C3 107.7(5) 23_655 23_655 ?
C2 N1 Zn1 111.9(5) . . ?
C2 N1 Zn1 111.9(5) 23_655 . ?
C2 N1 C2 62.2(8) . 23_655 ?
C3 N1 Zn1 111.0(5) . . ?
C3 N1 Zn1 111.0(5) 23_655 . ?
C3 N1 C2 106.3(5) . . ?
C3 N1 C2 106.3(5) 23_655 23_655 ?
C3 N1 C2 136.7(6) . 23_655 ?
C3 N1 C2 136.7(6) 23_655 . ?
C3 N1 C3 51.3(7) . 23_655 ?
N1 C1 C1 111.5(4) . 11_566 ?
N1 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
N1 C1 C3 89.2(5) . 25_666 ?
C1 C1 H1A 109.3 11_566 . ?
C1 C1 H1B 109.3 11_566 . ?
C1 C1 C3 46.7(6) 11_566 25_666 ?
H1A C1 H1B 108.0 . . ?
C3 C1 H1A 80.0 25_666 . ?
C3 C1 H1B 155.1 25_666 . ?
N1 C2 H2A 109.6 . . ?
N1 C2 H2B 109.6 . . ?
N1 C2 C3 110.1(6) . 11_566 ?
H2A C2 H2B 108.2 . . ?
C3 C2 H2A 109.6 11_566 . ?
C3 C2 H2B 109.6 11_566 . ?
N1 C3 C2 112.2(7) . 11_566 ?
N1 C3 H3A 109.2 . . ?
N1 C3 H3B 109.2 . . ?
C2 C3 H3A 109.2 11_566 . ?
C2 C3 H3B 109.2 11_566 . ?
H3A C3 H3B 107.9 . . ?
Zn2 O22 Zn1 121.5(2) . . ?
C22 O22 Zn1 115.8(9) . . ?
C22 O22 Zn2 119.3(8) . . ?
C23 O22 Zn1 111.4(8) 23_655 . ?
C23 O22 Zn2 127.0(8) 23_655 . ?
C23 O22 C22 24.0(4) 23_655 . ?
C24 O23 H23A 109.5 . . ?
O21 C21 H21A 109.0 . . ?
O21 C21 H21B 109.0 . . ?
O21 C21 C22 112.9(17) . . ?
H21A C21 H21B 107.8 . . ?
C22 C21 H21A 109.0 . . ?
C22 C21 H21B 109.0 . . ?
O22 C22 C21 110.8(13) . . ?
O22 C22 C23 105.4(12) . . ?
C21 C22 C23 103.1(12) . . ?
O22 C23 C22 110.7(14) 23_655 . ?
O22 C23 C24 122.4(15) 23_655 . ?
C24 C23 C22 101.1(11) . . ?
O23 C24 C23 115.6(17) . . ?
O23 C24 H24A 108.4 . . ?
O23 C24 H24B 108.4 . . ?
C23 C24 H24A 108.4 . . ?
C23 C24 H24B 108.4 . . ?
H24A C24 H24B 107.4 . . ?

_refine_diff_density_max         0.388
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.068




