Coordination-induced spontaneous resolution of a TPPE-based MOF and its use as a crystalline sponge in guest determination.
Cui, Ruoyu; Niu, Helin; Sheng, Enhong; Dalton transactions (Cambridge, England : 2003) 50 (2021) 7186–7190; doi:10.1039/d1dt00928a

data_7707332
_publ_section_title
;
 Coordination-induced spontaneous resolution of a TPPE-based MOF and its
 use as a crystalline sponge in guest determination.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7186
_journal_page_last               7190
_journal_paper_doi               10.1039/d1dt00928a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C46 H32 Cl2 Co N4, 4(C3 H7 N O)'
_chemical_formula_sum            'C58 H60 Cl2 Co N8 O4'
_chemical_formula_weight         1062.97
_space_group_crystal_system      orthorhombic
_space_group_IT_number           23
_space_group_name_Hall           'I 2 2'
_space_group_name_H-M_alt        'I 2 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-03-21 deposited with the CCDC.	2021-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.907(3)
_cell_length_b                   14.568(3)
_cell_length_c                   16.881(4)
_cell_measurement_reflns_used    1860
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.72
_cell_measurement_theta_min      2.80
_cell_volume                     2928.2(12)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7324
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.553
_diffrn_reflns_theta_min         1.846
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            deep-red
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             1114
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details
;
 Flack x determined using 891 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.116(17)
_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     167
_refine_ls_number_reflns         3350
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0596
_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^)+(0.1326P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1683
_refine_ls_wR_factor_ref         0.2031
_reflns_Friedel_coverage         0.778
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                2535
_reflns_number_total             3350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00928a2.cif
_cod_data_source_block           1M-DMF
_cod_depositor_comments
'Adding full bibliography for 7707332--7707338.cif.'
_cod_original_cell_volume        2928.1(11)
_cod_database_code               7707332
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C14
 1.52 with sigma of 0.02
 O1-C13
 1.27 with sigma of 0.02
 C14-N1 \\sim N1-C15
 with sigma of 0.01
 C15-N1 \\sim N1-C13
 with sigma of 0.01
 C14-N1 \\sim N1-C13
 with sigma of 0.01
 C15-C14 \\sim C14-C13
 with sigma of 0.02
 C14-C13 \\sim C13-C15
 with sigma of 0.02
 C13-C15 \\sim C15-C14
 with sigma of 0.02
3. Restrained planarity
 C13, O1, N1, C14, C15
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
O1 \\sim C13 \\sim N1 \\sim C14 \\sim C15: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
5.a Me refined with riding coordinates:
 C15(H15A,H15B,H15C), C14(H14A,H14B,H14C)
5.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C12(H12), C7(H7), C11(H11), C6(H6), C10(H10), C4(H4), C3(H3), C13(H13)
;
_shelx_res_checksum              13968
_olex2_submission_special_instructions 'No special instructions were received'