Coordination-induced conformation diversity for pharmaceutical polymorph control
Kang, Juan; Wang, Yongli; Chen, Yifu; Huang, Xin; Yin, Qiuxiang; Wang, Na; Hao, Hongxun; CrystEngComm 21 (2019) 6585–; doi:10.1039/C9CE01310E

data_7234202
_publ_section_title
;
 Coordination-induced conformation diversity for pharmaceutical polymorph
 control
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              6585
_journal_paper_doi               10.1039/C9CE01310E
_journal_volume                  21
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C40 H44 Cu4 N12 O12 S8, 2(C H4 O)'
_chemical_formula_sum            'C42 H52 Cu4 N12 O14 S8'
_chemical_formula_weight         1459.59
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-29 deposited with the CCDC.    2019-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.4476(3)
_cell_length_b                   10.10680(10)
_cell_length_c                   17.29590(10)
_cell_measurement_reflns_used    36041
_cell_measurement_temperature    300.99(10)
_cell_measurement_theta_max      74.5420
_cell_measurement_theta_min      2.7310
_cell_volume                     5672.04(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45g (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)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     22.00 118.00   0.50    0.15    --   46.12  79.00  32.00  192
  2  \w   -173.00 -84.00   0.50    0.58    -- -100.00 -55.00  33.00  178
  3  \w   -125.00 -27.00   0.50    0.58    -- -100.00  79.00  32.00  196
  4  \w     29.00 132.00   0.50    0.58    --  101.75 -91.00 167.00  206
  5  \w     32.00 120.00   0.50    0.15    --   46.12  38.00 150.00  176
  6  \w     20.00  95.00   0.50    0.15    --   46.12-125.00-120.00  150
  7  \w   -172.00 -85.00   0.50    0.58    -- -100.00 -45.00 -60.00  174
  8  \w   -115.00 -25.00   0.50    0.58    -- -100.00  30.00-180.00  180
  9  \w   -176.00 -82.00   0.50    0.58    -- -100.00 -15.00 -60.00  188
 10  \w     84.00 178.00   0.50    0.58    --  101.75  15.00 150.00  188
 11  \w     87.00 174.00   0.50    0.58    --  101.75  45.00   0.00  174
 12  \w     30.00 118.00   0.50    0.15    --   46.12  57.00-120.00  176
 13  \w     30.00 118.00   0.50    0.15    --   46.12  57.00-180.00  176
 14  \w     23.00 118.00   0.50    0.15    --   46.12  77.00 -60.00  190
 15  \w     86.00 117.00   0.50    0.58    --  101.75  30.00-150.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0073223000
_diffrn_orient_matrix_UB_12      0.1133645000
_diffrn_orient_matrix_UB_13      -0.0579098000
_diffrn_orient_matrix_UB_21      0.0301725000
_diffrn_orient_matrix_UB_22      -0.0653915000
_diffrn_orient_matrix_UB_23      -0.0571667000
_diffrn_orient_matrix_UB_31      -0.0359087000
_diffrn_orient_matrix_UB_32      -0.0781746000
_diffrn_orient_matrix_UB_33      -0.0362390000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49960
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.660
_diffrn_reflns_theta_min         2.724
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.062
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_description       block
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 4245 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         10667
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0289
_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/[\s^2^(Fo^2^)+(0.0470P)^2^+1.3875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0778
_reflns_Friedel_coverage         0.827
_reflns_Friedel_fraction_full    0.920
_reflns_Friedel_fraction_max     0.860
_reflns_number_gt                9979
_reflns_number_total             10667
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01310e2.cif
_cod_data_source_block           kj-19
_cod_depositor_comments
'Adding full bibliography for 7234202--7234204.cif.'
_cod_database_code               7234202
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.517
_shelx_estimated_absorpt_t_min   0.431
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Rotating group:
 N2(H2A,H2B), N4(H4A,H4B), N1(H1A,H1B), N3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C18(H18), C17(H17), C35(H35), C23(H23), C14(H14), C5(H5), C24(H24),
 C34(H34), C28(H28), C19(H19), C31(H31), C8(H8), C29(H29), C12(H12), C9(H9),
 C2(H2), C32(H32), C26(H26), C6(H6), C20(H20), C13(H13), C3(H3), C11(H11)
2.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C38(H38A,H38B,H38C), C37(H37A,H37B,H37C), C41(H41A,H41B,
 H41C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
2.d Idealised tetrahedral OH refined as rotating group:
 O14(H14A), O13(H13A)
;
_shelx_res_checksum              92009
_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 2.232
_oxdiff_exptl_absorpt_empirical_full_min 0.631