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_1565816
_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 Co2 N8, C H2 Cl2'
_chemical_formula_sum            'C77 H80 Cl4 Co2 N8'
_chemical_formula_weight         1377.15
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-14
_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                 100.8950(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.3373(6)
_cell_length_b                   14.5574(3)
_cell_length_c                   20.3283(5)
_cell_measurement_reflns_used    9823
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      63.62
_cell_measurement_theta_min      3.18
_cell_volume                     8234.6(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      173.0
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50287
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        63.857
_diffrn_reflns_theta_max         63.857
_diffrn_reflns_theta_min         3.176
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.669
_exptl_absorpt_correction_T_max  0.7524
_exptl_absorpt_correction_T_min  0.4468
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1301 before and 0.0568 after correction.
The Ratio of minimum to maximum transmission is 0.5938.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Cyan
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_description       needle
_exptl_crystal_F_000             2880
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         13406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0583
_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^)+(0.1105P)^2^+3.6181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1701
_refine_ls_wR_factor_ref         0.1810
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10626
_reflns_number_total             13406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06514a2.cif
_cod_data_source_block           ta_a_sq_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1565814--1565817.cif.'
_cod_database_code               1565816
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a 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), C77(H77A,H77B)
2.b 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)
2.c 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)
;
_shelx_res_checksum              25002
_shelx_hkl_checksum              33981
_shelx_fab_checksum              6050
_olex2_submission_special_instructions 'No special instructions were received'