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_7707334
_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_absolute_configuration ad
_chemical_formula_moiety         'C46 H32 Cl2 Co N4, 4(C4 H11 N)'
_chemical_formula_sum            'C62 H76 Cl2 Co N8'
_chemical_formula_weight         1063.13
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-04-30 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                   11.8964(16)
_cell_length_b                   14.5101(19)
_cell_length_c                   17.098(2)
_cell_measurement_reflns_used    2387
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.33
_cell_measurement_theta_min      2.38
_cell_volume                     2951.4(7)
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0293
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6820
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.501
_diffrn_reflns_theta_min         1.841
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            deep-red
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             1130
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Flack x determined using 950 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         3363
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.217
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0590
_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^)+(0.1243P)^2^+0.6565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1737
_refine_ls_wR_factor_ref         0.1899
_reflns_Friedel_coverage         0.758
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.965
_reflns_number_gt                2640
_reflns_number_total             3363
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00928a2.cif
_cod_data_source_block           1P-S-2-butylamine
_cod_depositor_comments
'Adding full bibliography for 7707332--7707338.cif.'
_cod_database_code               7707334
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C15
 1.47 with sigma of 0.01
 C14-C13
 1.53 with sigma of 0.01
 C15-C14
 1.53 with sigma of 0.01
 C16-C15
 1.53 with sigma of 0.01
 H14A-H14A_$1
 2.2 with sigma of 0.02
 H1A-H1A_$1
 2.4 with sigma of 0.02
 H4-H13A
 2.6 with sigma of 0.02
 H13B_$1-H16C
 2.4 with sigma of 0.02
 C15-C13
 2.48 with sigma of 0.01
 C16-C14
 2.48 with sigma of 0.01
 C16-C14 \\sim C15-C13
 with sigma of 0.02
 C14-N1 \\sim N1-C16
 with sigma of 0.02
3. Rigid bond restraints
 C13, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C13 \\sim C16: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
5.a Riding coordinates:
 C13(H13A,H13B,H13C), N1(H1A,H1B)
5.b Ternary CH refined with riding coordinates:
 C15(H15)
5.c Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B)
5.d Me refined with riding coordinates:
 C16(H16A,H16B,H16C)
5.e Aromatic/amide H refined with riding coordinates:
 C12(H12), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C7(H7), C6(H6)
;
_shelx_res_checksum              20624
_olex2_submission_special_instructions 'No special instructions were received'