Interplay between the crystal stability and the energy of the molecular conformation
Dyk, Konrad; Baran, Łukasz; Rżysko, Wojciech; Stankevič, Marek; Kamiński, Daniel M.; CrystEngComm 23 (2021) 2683–2694; doi:10.1039/D0CE01673J

data_7242306
_publ_section_title
;
 Interplay between the crystal stability and the energy of the molecular
 conformation
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2683
_journal_page_last               2694
_journal_paper_doi               10.1039/D0CE01673J
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C24 H18 O4, 2[H2O]'
_chemical_formula_sum            'C24 H18 O4'
_chemical_formula_weight         370.38
_chemical_melting_point          523
_chemical_name_common            BHDB
_chemical_name_systematic
5,5?-bis(4-hydroxyphenyl)-2,2?-dihydroxy-1,1?-biphenyl
_space_group_crystal_system      cubic
_space_group_IT_number           228
_space_group_name_Hall           '-F 4ud 2vw 3'
_space_group_name_H-M_alt        'F d -3 c :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc27617r
_audit_creation_date             2021-02-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257)
;
_audit_update_record
;
2021-02-17 deposited with the CCDC.	2021-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            96
_cell_length_a                   36.4661(5)
_cell_length_b                   36.4661(5)
_cell_length_c                   36.4661(5)
_cell_measurement_reflns_used    20403
_cell_measurement_temperature    293.0
_cell_measurement_theta_max      66.8220
_cell_measurement_theta_min      4.1800
_cell_volume                     48491.8(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_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     19.00  82.00   0.50   10.00    --    0.00  30.00 -60.00  126
  2  \w    -83.00  81.00   0.50   20.00    --    5.00  30.00  90.00  328
  3  \w   -141.00-115.00   0.50   20.00    --  -90.00  60.00  16.14   52
  4  \w    -52.00  -2.00   0.50   20.00    --  -90.00  60.00  16.14  100
  5  \w   -158.00 -84.00   0.50   20.00    --  -90.00  59.00 -26.53  148
  6  \w    -44.00 -18.00   0.50   20.00    --  -90.00  59.00 -26.53   52
  7  \w   -178.00 -96.00   0.50   20.00    --  -90.00  50.00 150.00  164
  8  \w   -176.00 -57.00   0.50   20.00    --  -90.00  60.00  35.03  238
  9  \w    -76.00  -3.00   0.50   20.00    --  -90.00  50.00 150.00  146
 10  \w   -148.00 -79.00   0.50   20.00    --  -90.00  59.00  83.24  138
 11  \w    -72.00  -8.00   0.50   20.00    --  -90.00  59.00  83.24  128
 12  \w   -179.00-122.00   0.50   20.00    --  -90.00  40.00 -90.00  114
 13  \w   -109.00 -83.00   0.50   20.00    --  -90.00  40.00 -90.00   52
 14  \w   -171.00-119.00   0.50   20.00    --  -90.00  60.00 164.09  104
 15  \w   -105.00 -46.00   0.50   20.00    --  -90.00  60.00 164.09  118
 16  \w    -88.00 -62.00   0.50   20.00    --  -90.00  60.00  16.14   52
 17  \w    -50.00  -2.00   0.50   20.00    --  -90.00  60.00  35.03   96
 18  \w    -58.00 -22.00   0.50   20.00    --  -90.00  60.00-125.08   72
 19  \w   -179.00-114.00   0.50   20.00    --  -90.00  60.00 -59.58  130
 20  \w    -58.00  -3.00   0.50   20.00    --  -90.00  60.00 -59.58  110
 21  \w   -134.00  -2.00   0.50   20.00    --  -90.00  20.00-120.00  264
 22  \w   -175.00-142.00   0.50   20.00    --  -90.00  60.00  97.15   66
 23  \w   -118.00 -93.00   0.50   20.00    --  -90.00  60.00  97.15   50
 24  \w    -60.00  -7.00   0.50   20.00    --  -90.00  60.00  97.15  106
 25  \w    -56.00  -5.00   0.50   20.00    --  -90.00  40.00 120.00  102
 26  \w   -152.00-127.00   0.50   20.00    --  -90.00  10.00 -90.00   50
 27  \w    -51.00 -10.00   0.50   20.00    --  -90.00  10.00 -90.00   82
 28  \w    -93.00 -67.00   0.50   20.00    --  -90.00  40.00 -60.00   52
 29  \w   -174.00-149.00   0.50   20.00    --  -90.00  60.00-171.63   50
 30  \w    -47.00 -22.00   0.50   20.00    --  -90.00  60.00-171.63   50
 31  \w   -176.00 -77.00   0.50   20.00    --  -90.00  60.00-125.08  198
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0158972000
_diffrn_orient_matrix_UB_12      0.0279869000
_diffrn_orient_matrix_UB_13      -0.0273768000
_diffrn_orient_matrix_UB_21      -0.0376719000
_diffrn_orient_matrix_UB_22      -0.0029541000
_diffrn_orient_matrix_UB_23      0.0189039000
_diffrn_orient_matrix_UB_31      0.0106070000
_diffrn_orient_matrix_UB_32      0.0314925000
_diffrn_orient_matrix_UB_33      0.0260683000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            125860
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.766
_diffrn_reflns_theta_min         3.428
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       cube
_exptl_crystal_F_000             18624
_exptl_crystal_preparation
'milling with acetonitrille and trimesic acid, recrystallization from acetonitrille, acetic acid solution 1:1'
_exptl_crystal_recrystallization_method evaporation
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.140
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1872
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0537
_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/[\s^2^(Fo^2^)+(0.1069P)^2^+19.1381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1678
_refine_ls_wR_factor_ref         0.1811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1441
_reflns_number_total             1872
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01673j1.cif
_cod_data_source_block           dhbd
_cod_depositor_comments
'Adding full bibliography for 7242306--7242309.cif.'
_cod_original_cell_volume        48492(2)
_cod_original_sg_symbol_Hall     '-F 4cvw 2vw 3'
_cod_original_sg_symbol_H-M      'F d -3 c'
_cod_database_code               7242306
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     '0.2 x 0.2 x 0'
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.878
_reflns_odcompleteness_completeness 98.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.01
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H3O), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11), C12(H12)
2.b Idealised tetrahedral OH refined as rotating group:
 O1(H1O), O2(H2O)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              95320
_shelx_fab_checksum              87320
_olex2_exptl_crystal_mounting_method oil
_olex2_submission_original_sample_id BHDB
_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 1.584
_oxdiff_exptl_absorpt_empirical_full_min 0.792