Guest-Binding-Induced Interhetero Hosts Charge Transfer Crystallization: Selective Coloration of Commonly Used Organic Solvents.
Mi, Yan; Ma, Jingyu; Liang, Wenting; Xiao, Chao; Wu, Wanhua; Zhou, Dayang; Yao, Jiabin; Sun, Wenjia; Sun, Junliang; Gao, Guowei; Chen, Xiaochuan; Chruma, Jason J.; Yang, Cheng; Journal of the American Chemical Society 143 (2021) 1553–1561; doi:10.1021/jacs.0c11833

data_4135616
_publ_section_title
;
 Guest-Binding-Induced Interhetero Hosts Charge Transfer Crystallization:
 Selective Coloration of Commonly Used Organic Solvents.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1553
_journal_page_last               1561
_journal_paper_doi               10.1021/jacs.0c11833
_journal_volume                  143
_journal_year                    2021
_chemical_formula_moiety      'C45 H50 O10, C35 H20 O10, 2(C2 H4 O2), C4 H7 O2'
_chemical_formula_sum            'C88 H86 O24'
_chemical_formula_weight         1527.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-11-29
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_cell_angle_alpha                68.21
_cell_angle_beta                 89.91
_cell_angle_gamma                73.20
_cell_formula_units_Z            2
_cell_length_a                   12.182
_cell_length_b                   17.093
_cell_length_c                   21.861
_cell_measurement_reflns_used    15326
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.4850
_cell_measurement_theta_min      2.1800
_cell_volume                     4017.687
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  ' '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            58741
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.726
_diffrn_reflns_theta_min         1.010
_exptl_absorpt_coefficient_mu    0.092
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       ' '
_exptl_crystal_F_000             1612
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1043
_refine_ls_number_reflns         16259
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      49.204
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0731
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1278P)^2^+1.3052P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2179
_refine_ls_wR_factor_ref         0.2400
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11227
_reflns_number_total             16259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11833_si_002.cif
_cod_data_source_block           08
_cod_depositor_comments
;

2025-09-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C176 H172 O48'
_cod_original_formula_weight         3055.13
_cod_original_formula_moiety
'2(C45 H50 O10), 2(C35 H20 O10), 4(C2 H4 O2), 2(C4 H7 O2)'
_cod_original_formula_units_Z            1
_cod_original_cell_volume        4017.6
_cod_database_code               4135616
_shelx_shelxl_version_number     2018/3
_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, All O(H) groups
2. Restrained distances
 C88-C89
 1.42 with sigma of 0.005
 O26-O23
 2.04 with sigma of 0.001
 C7-O13 \\sim C71-O5 \\sim C88-O26
 with sigma of 0.001
 C85-O26 \\sim C89-O26
 with sigma of 0.001
3.a Secondary CH2 refined with riding coordinates:
 C10(H10a,H10b), C31(H31a,H31b), C35(H35a,H35b), C36(H36a,H36b), C37(H37a,
 H37b), C44(H44a,H44b), C45(H45a,H45b), C49(H49a,H49b), C70(H70a,H70b),
 C72(H72a,H72b)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C16(H16), C17(H17), C20(H20), C26(H26), C27(H27), C32(H32), C39(H39),
 C40(H40), C41(H41), C42(H42), C43(H43), C51(H51), C52(H52), C54(H54), C58(H58),
  C60(H60), C64(H64), C67(H67), C68(H68), C88(H88)
3.c Idealised Me refined as rotating group:
 C69(H69a,H69b,H69c), C71(H71a,H71b,H71c), C73(H73a,H73b,H73c), C74(H74a,H74b,
 H74c), C75(H75a,H75b,H75c), C76(H76a,H76b,H76c), C77(H77a,H77b,H77c), C79(H79a,
 H79b,H79c), C80(H80a,H80b,H80c), C83(H83a,H83b,H83c), C84(H84a,H84b,H84c),
 C85(H85a,H85b,H85c), C87(H87a,H87b,H87c), C89(H89a,H89b,H89c)
3.d Idealised tetrahedral OH refined as rotating group:
 O22(H22), O24(H24)
;
_shelx_res_checksum              67024
_shelx_hkl_checksum              66148
_olex2_submission_special_instructions 'No special instructions were received'