data_ca147m
_audit_creation_date               2018-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_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. (2008). Acta Cryst. A64, 112-122.
;
_chemical_name_common              ?
_chemical_name_systematic
;
 ? 
;
_chemical_formula_moiety           '2(C30 H32 O6)'
_chemical_formula_sum              'C60 H64 O12'
_chemical_formula_weight           977.11
_chemical_melting_point            ?
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'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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_id
  _space_group_symop_operation_xyz
 1 'x, y, z'
 2 '-x+1/2, y+1/2, -z+1/2'
 3 '-x, -y, -z'
 4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                     5.1831(6)
_cell_length_b                     16.4627(19)
_cell_length_c                     14.3407(16)
_cell_angle_alpha                  90.00
_cell_angle_beta                   91.332(2)
_cell_angle_gamma                  90.00
_cell_volume                       1223.3(2)
_cell_formula_units_Z              1
_cell_measurement_reflns_used      2076
_cell_measurement_temperature      273
_cell_measurement_theta_max        26.305
_cell_measurement_theta_min        2.474
_exptl_absorpt_coefficient_mu      0.092
_exptl_absorpt_correction_T_max    0.9999
_exptl_absorpt_correction_T_min    0.685252
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0423 before and 0.0204 after correction.
The Ratio of minimum to maximum transmission is 0.6853.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour              'metallic light colourless'
_exptl_crystal_colour_lustre       metallic
_exptl_crystal_colour_modifier     light
_exptl_crystal_colour_primary      colourless
_exptl_crystal_density_diffrn      1.326
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         block
_exptl_crystal_F_000               520
_exptl_crystal_preparation         ?
_exptl_crystal_recrystallization_method  ?
_exptl_crystal_size_max            0.001
_exptl_crystal_size_mid            0.001
_exptl_crystal_size_min            0.001
_exptl_special_details
;
 ? 
;
_diffrn_reflns_av_R_equivalents    0.0241
_diffrn_reflns_av_unetI/netI       0.0300
_diffrn_reflns_limit_h_max         4
_diffrn_reflns_limit_h_min         -6
_diffrn_reflns_limit_k_max         20
_diffrn_reflns_limit_k_min         -20
_diffrn_reflns_limit_l_max         17
_diffrn_reflns_limit_l_min         -16
_diffrn_reflns_number              6886
_diffrn_reflns_theta_full          26.40
_diffrn_reflns_theta_max           26.40
_diffrn_reflns_theta_min           1.88
_diffrn_ambient_temperature        273.0
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.997
_diffrn_measured_fraction_theta_max  0.997
_diffrn_measurement_device_type    'CCD Area Detector'
_diffrn_measurement_method         ?
_diffrn_radiation_monochromator    graphite
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'fine-focus sealed tube'
_diffrn_standards_decay_%          ?
_diffrn_standards_interval_count   ?
_diffrn_standards_interval_time    ?
_diffrn_standards_number           ?
_reflns_number_gt                  1921
_reflns_number_total               2506
_reflns_threshold_expression       >2sigma(I)
_computing_cell_refinement         'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection         ?
_computing_data_reduction          'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'XL (Sheldrick, 2008)'
_computing_structure_solution      'XS (Sheldrick, 2008)'
_refine_diff_density_max           0.252
_refine_diff_density_min           -0.172
_refine_diff_density_rms           0.042
_refine_ls_extinction_coef         ?
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.035
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       166
_refine_ls_number_reflns           2506
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0595
_refine_ls_R_factor_gt             0.0439
_refine_ls_restrained_S_all        1.035
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'calc w=1/[σ²(Fo²)+(0.0592P)²+0.3080P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1103
_refine_ls_wR_factor_ref           0.1198
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_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)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C10(H10), C13(H13), C16(H16)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary       direct
_atom_sites_solution_secondary     difmap
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_calc_flag
  _atom_site_disorder_assembly
  _atom_site_disorder_group
  _atom_site_refinement_flags_posn
 O1 O 0.2181(2) 0.30269(7) 0.22486(8) 0.0397(3) Uani 1 d . . .
 O2 O -0.3869(2) 0.20330(7) 0.00644(8) 0.0385(3) Uani 1 d . . .
 C3 C 0.1943(3) 0.15722(9) 0.20290(11) 0.0311(4) Uani 1 d . . .
 H3 H 0.3272 0.1482 0.2463 0.037 Uiso 1 calc . . R
 O4 O 0.1405(3) 0.01347(7) 0.17281(9) 0.0464(4) Uani 1 d . . .
 C5 C 0.1582(3) 0.35645(9) -0.01879(11) 0.0313(4) Uani 1 d . . .
 H5 H 0.1878 0.3008 -0.0161 0.038 Uiso 1 calc . . R
 C6 C -0.0870(3) 0.25188(9) 0.11764(11) 0.0287(4) Uani 1 d . . .
 C7 C 0.1108(3) 0.23566(9) 0.18204(11) 0.0298(4) Uani 1 d . . .
 C8 C 0.0740(3) 0.09317(9) 0.15725(12) 0.0331(4) Uani 1 d . . .
 C9 C -0.1827(3) 0.33771(9) 0.10151(12) 0.0317(4) Uani 1 d . . .
 H9A H -0.1868 0.3651 0.1614 0.038 Uiso 1 calc . . R
 H9B H -0.3589 0.3349 0.0774 0.038 Uiso 1 calc . . R
 C10 C -0.1217(3) 0.10583(9) 0.09112(12) 0.0331(4) Uani 1 d . . .
 H10 H -0.2000 0.0622 0.0606 0.040 Uiso 1 calc . . R
 C11 C -0.0754(3) 0.47553(9) 0.03007(10) 0.0270(3) Uani 1 d . . .
 C12 C -0.1983(3) 0.18488(9) 0.07143(11) 0.0298(4) Uani 1 d . . .
 C13 C 0.3054(3) 0.40453(10) -0.07854(12) 0.0355(4) Uani 1 d . . .
 H13 H 0.4303 0.3804 -0.1149 0.043 Uiso 1 calc . . R
 C14 C 0.4174(4) 0.29027(11) 0.29310(13) 0.0397(4) Uani 1 d . . .
 H14A H 0.5601 0.2632 0.2651 0.060 Uiso 1 calc . . GR
 H14B H 0.3532 0.2574 0.3428 0.060 Uiso 1 calc . . GR
 H14C H 0.4734 0.3418 0.3175 0.060 Uiso 1 calc . . GR
 C15 C -0.0277(3) 0.38970(9) 0.03553(10) 0.0277(4) Uani 1 d . . .
 C16 C 0.2667(3) 0.48634(10) -0.08368(11) 0.0328(4) Uani 1 d . . .
 H16 H 0.3673 0.5175 -0.1229 0.039 Uiso 1 calc . . R
 C17 C -0.5142(4) 0.13760(12) -0.03979(14) 0.0459(5) Uani 1 d . . .
 H17A H -0.6382 0.1585 -0.0844 0.069 Uiso 1 calc . . GR
 H17B H -0.6007 0.1048 0.0052 0.069 Uiso 1 calc . . GR
 H17C H -0.3895 0.1051 -0.0713 0.069 Uiso 1 calc . . GR
 C18 C 0.3404(4) -0.00035(11) 0.24138(14) 0.0478(5) Uani 1 d . . .
 H18A H 0.4980 0.0238 0.2210 0.072 Uiso 1 calc . . GR
 H18B H 0.3648 -0.0577 0.2497 0.072 Uiso 1 calc . . GR
 H18C H 0.2924 0.0237 0.2995 0.072 Uiso 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
 O1 C7 1.3740(19) . ?
 O1 C14 1.421(2) . ?
 O2 C12 1.3689(19) . ?
 O2 C17 1.423(2) . ?
 C3 C7 1.392(2) . ?
 C3 C8 1.382(2) . ?
 O4 C8 1.3735(19) . ?
 O4 C18 1.430(2) . ?
 C5 C13 1.405(2) . ?
 C5 C15 1.367(2) . ?
 C6 C7 1.390(2) . ?
 C6 C9 1.513(2) . ?
 C6 C12 1.404(2) . ?
 C8 C10 1.388(2) . ?
 C9 C15 1.520(2) . ?
 C10 C12 1.388(2) . ?
 C11 C11 1.427(3) 3_565 ?
 C11 C15 1.436(2) . ?
 C11 C16 1.415(2) 3_565 ?
 C13 C16 1.363(2) . ?
 C16 C11 1.415(2) 3_565 ?

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
 C7 O1 C14 118.18(12) . . ?
 C12 O2 C17 117.70(13) . . ?
 C8 C3 C7 118.13(15) . . ?
 C8 O4 C18 116.02(13) . . ?
 C15 C5 C13 121.46(14) . . ?
 C7 C6 C9 121.00(14) . . ?
 C7 C6 C12 116.84(14) . . ?
 C12 C6 C9 122.12(14) . . ?
 O1 C7 C3 121.91(14) . . ?
 O1 C7 C6 115.29(13) . . ?
 C6 C7 C3 122.80(14) . . ?
 C3 C8 C10 121.56(14) . . ?
 O4 C8 C3 122.90(15) . . ?
 O4 C8 C10 115.53(14) . . ?
 C6 C9 C15 116.42(13) . . ?
 C12 C10 C8 118.75(15) . . ?
 C11 C11 C15 119.51(17) 3_565 . ?
 C16 C11 C11 118.58(17) 3_565 3_565 ?
 C16 C11 C15 121.91(14) 3_565 . ?
 O2 C12 C6 115.25(13) . . ?
 O2 C12 C10 122.87(14) . . ?
 C10 C12 C6 121.88(15) . . ?
 C16 C13 C5 120.55(15) . . ?
 C5 C15 C9 121.28(14) . . ?
 C5 C15 C11 119.04(14) . . ?
 C11 C15 C9 119.68(13) . . ?
 C13 C16 C11 120.85(15) . 3_565 ?


_olex2_submission_special_instructions  'No special instructions were received'
