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_7242308
_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'
_chemical_formula_sum            'C24 H18 O4'
_chemical_formula_weight         370.38
_chemical_melting_point          523
_chemical_name_common            DHBD
_chemical_name_systematic
5,5?-bis(4-hydroxyphenyl)-2,2?-dihydroxy-1,1?-biphenyl
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc27819w
_audit_creation_date             2021-02-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-02-16 deposited with the CCDC.	2021-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.154(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3982(4)
_cell_length_b                   8.72673(20)
_cell_length_c                   9.6682(2)
_cell_measurement_reflns_used    3684
_cell_measurement_temperature    120.10(10)
_cell_measurement_theta_max      75.5090
_cell_measurement_theta_min      4.3610
_cell_volume                     1714.07(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.10(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2763
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_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     25.00  59.00   1.00    2.25    --   40.94  37.00  60.00   34
  2  \w     83.00 114.00   1.00    2.25    --   40.94  37.00  60.00   31
  3  \w     44.00  95.00   1.00    9.00    --  112.00 -61.00  90.00   51
  4  \w    114.00 139.00   1.00    9.00    --  112.00 -61.00  90.00   25
  5  \w     71.00 110.00   1.00    9.00    --  112.00-111.00  30.00   39
  6  \w     58.00  97.00   1.00    9.00    --  112.00 -94.00  90.00   39
  7  \w     44.00 137.00   1.00    9.00    --  112.00 -45.00 -30.00   93
  8  \w     83.00 136.00   1.00    9.00    --  112.00  61.00-120.00   53
  9  \w     96.00 148.00   1.00    9.00    --  112.00 111.00  60.00   52
 10  \w     47.00  84.00   1.00    9.00    --  112.00 -61.00 -60.00   37
 11  \w     37.00  63.00   1.00    9.00    --  112.00-111.00  30.00   26
 12  \w     29.00  54.00   1.00    9.00    --  112.00 -94.00 -30.00   25
 13  \w     40.00 109.00   1.00    9.00    --  112.00 -94.00 -90.00   69
 14  \w     84.00 116.00   1.00    9.00    --  112.00-111.00-180.00   32
 15  \w     38.00  64.00   1.00    9.00    --  112.00-111.00-180.00   26
 16  \w     26.00 155.00   1.00    9.00    --  112.00   0.00-120.00  129
 17  \w     41.00  90.00   1.00    9.00    --  112.00 -61.00 150.00   49
 18  \w     11.00  98.00   1.00    2.25    --   40.94  77.00  90.00   87
 19  \w     13.00 110.00   1.00    2.25    --   40.94  57.00-150.00   97
 20  \w    -69.00  32.00   1.00    2.25    --  -40.94  57.00 -30.00  101
 21  \w    -95.00 -65.00   1.00    2.25    --  -40.94 125.00 -90.00   30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0454535000
_diffrn_orient_matrix_UB_12      -0.1237479000
_diffrn_orient_matrix_UB_13      -0.0527232000
_diffrn_orient_matrix_UB_21      -0.0033987000
_diffrn_orient_matrix_UB_22      0.0798132000
_diffrn_orient_matrix_UB_23      -0.1426867000
_diffrn_orient_matrix_UB_31      0.0605873000
_diffrn_orient_matrix_UB_32      0.0974318000
_diffrn_orient_matrix_UB_33      0.0495640000
_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  0.0201
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5339
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.230
_diffrn_reflns_theta_min         4.353
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.790
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       plate
_exptl_crystal_F_000             776
_exptl_crystal_preparation       'Evaporation from acetonitrille'
_exptl_crystal_recrystallization_method 'crystallization from acetonitrille'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         1766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0481P)^2^+1.4506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.0975
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1655
_reflns_number_total             1766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01673j1.cif
_cod_data_source_block           konrad_120k
_cod_depositor_comments
'Adding full bibliography for 7242306--7242309.cif.'
_cod_original_cell_volume        1714.08(6)
_cod_database_code               7242308
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C12H6O2
_chemical_oxdiff_usercomment     'Kryszta Konrada 120K'
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.743
_reflns_odcompleteness_completeness 99.88
_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:
 C12(H12), C11(H11), C4(H4), C2(H2A), C9(H9), C8(H8), C5(H5)
2.b Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              6273
_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 1.588
_oxdiff_exptl_absorpt_empirical_full_min 0.486