An investigation of the selectivity behaviour of host compound (R,R)-(−)-2,3-dimethoxy-1,1,4,4-tetraphenylbutane-1,4-diol in mixed cresols
Barton, Benita; Pohl, Pieter L.; Hosten, Eric C.; CrystEngComm 25 (2023) 1731–1739; doi:10.1039/D3CE00101F

data_7246383
_publ_section_title
;
 An investigation of the selectivity behaviour of host compound
 (R,R)-(&#x2212;)-2,3-dimethoxy-1,1,4,4-tetraphenylbutane-1,4-diol in
 mixed cresols
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              1731
_journal_page_last               1739
_journal_paper_doi               10.1039/D3CE00101F
_journal_volume                  25
_journal_year                    2023
_chemical_absolute_configuration syn
_chemical_formula_moiety         '2(C30 H30 O4), C7 H8 O'
_chemical_formula_sum            'C67 H68 O9'
_chemical_formula_weight         1017.21
_chemical_melting_point          360.65
_chemical_name_common
;
2DMT/p-cresol
;
_chemical_name_systematic
;
(R,R)-(-)-2,3-dimethoxy-1,1,4,4-tetraphenylbutane-1,4-diol
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-02-01 deposited with the CCDC.	2023-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.152(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.3436(12)
_cell_length_b                   12.0126(8)
_cell_length_c                   14.0767(10)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.34
_cell_volume                     2753.2(3)
_computing_cell_refinement       'APEX2 v2011.4-1 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2011.4.0.0'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2012)'
_computing_publication_material
'PLATON (Spek, 2009) and MERCURY (Macrae, 2008)'
_computing_structure_refinement
'SHELXL-2018/3 (Sheldrick, 2015) and ShelXle (H\"ubschle, 2011)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28811
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.304
_diffrn_reflns_theta_min         2.107
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9411
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS-2008/1 (Bruker AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1084
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: p-cresol'
_exptl_crystal_size_max          0.661
_exptl_crystal_size_mid          0.613
_exptl_crystal_size_min          0.266
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.143
_refine_diff_density_rms         0.029
_refine_ls_abs_structure_details
;
 Flack x determined using 2659 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(19)
_refine_ls_extinction_coef       0.0025(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         6817
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0479P)^2^+0.4692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.905
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                6125
_reflns_number_total             6817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00101f2.cif
_cod_data_source_block           ha039
_cod_depositor_comments
'Adding full bibliography for 7246381--7246383.cif.'
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7246383
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.949
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              40067