Kinetic trapping of a cobalt(ii) metallocage using a carbazole-containing expanded carbaporphyrinoid ligand
Zhou, Weinan; Sarma, Tridib; Su, Yonghuan; Lei, Chuanhu; Sessler, Jonathan L.; Chemical Science 13 (2022) 692–697; doi:10.1039/D1SC06514A

data_1565815
_publ_section_title
;
 Kinetic trapping of a cobalt(ii) metallocage using a carbazole-containing
 expanded carbaporphyrinoid ligand
;
_journal_issue                   3
_journal_name_full               'Chemical Science'
_journal_page_first              692
_journal_page_last               697
_journal_paper_doi               10.1039/D1SC06514A
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C76 H78 Cl2 N8 Zn2, 2(C H Cl3), 3(C H4 O)'
_chemical_formula_sum            'C81 H92 Cl8 N8 O3 Zn2'
_chemical_formula_weight         1639.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-25 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.36(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.535(6)
_cell_length_b                   13.861(3)
_cell_length_c                   20.682(4)
_cell_measurement_reflns_used    69159
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      0.39
_cell_volume                     8020(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28063
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.160
_diffrn_reflns_theta_min         1.846
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.917
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       needle
_exptl_crystal_F_000             3416
_refine_diff_density_max         1.727
_refine_diff_density_min         -1.649
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     936
_refine_ls_number_reflns         17044
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0931
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1901P)^2^+4.7169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2829
_refine_ls_wR_factor_ref         0.3013
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13455
_reflns_number_total             17044
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06514a2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 1565814--1565817.cif.'
_cod_database_code               1565815
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C81) \\sim Ueq, Uanis(Cl7) \\sim Ueq, Uanis(Cl8) \\sim Ueq, Uanis(Cl6)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Riding coordinates:
 O1(H1)
3.b Ternary CH refined with riding coordinates:
 C80(H80), C81(H81)
3.c Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C14(H14A,H14B), C16(H16A,H16B), C23(H23A,H23B),
 C25(H25A,H25B), C43(H43A,H43B), C45(H45A,H45B), C52(H52A,H52B), C54(H54A,H54B),
  C61(H61A,H61B), C63(H63A,H63B)
3.d Aromatic/amide H refined with riding coordinates:
 N4(H4), N8(H8), C9(H9), C18(H18), C28(H28), C29(H29), C32(H32), C33(H33),
 C35(H35), C38(H38), C47(H47), C56(H56), C66(H66), C67(H67), C70(H70), C71(H71),
  C73(H73), C76(H76)
3.e Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C),
 C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C44(H44A,H44B,H44C), C46(H46A,H46B,
 H46C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C62(H62A,H62B,H62C), C64(H64A,
 H64B,H64C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C)
3.f Idealised tetrahedral OH refined as rotating group:
 O2(H2), O3(H3)
;
_shelx_res_checksum              10467
_shelx_hkl_checksum              73228
_olex2_submission_special_instructions 'No special instructions were received'