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_1565814
_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 H79 Co2 N8 O, 1.167(Cl), C H Cl3, 0.667(H2 O)'
_chemical_formula_sum            'C77 H81.33 Cl4.17 Co2 N8 O1.67'
_chemical_formula_weight         1411.06
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-08-25 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   31.1312(4)
_cell_length_b                   31.1312(4)
_cell_length_c                   15.5307(3)
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      67.11
_cell_measurement_theta_min      2.84
_cell_volume                     13035.1(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0842
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            165078
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.408
_diffrn_reflns_theta_min         2.839
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.496
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5525
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1002 before and 0.0763 after correction.
The Ratio of minimum to maximum transmission is 0.7336.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            DarkCyan
_exptl_crystal_density_diffrn    1.079
_exptl_crystal_description       block
_exptl_crystal_F_000             4425
_exptl_crystal_preparation       'Magnetic properties'
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     853
_refine_ls_number_reflns         15952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0605
_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^)+(0.0976P)^2^+11.8377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.1820
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12191
_reflns_number_total             15952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06514a2.cif
_cod_data_source_block           ta_a_sq
_cod_depositor_comments
'Adding full bibliography for 1565814--1565817.cif.'
_cod_original_cell_volume        13035.1(4)
_cod_database_code               1565814
_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, All O(H,H) groups
2. Others
 Fixed Sof: H2A(0.33333) H2B(0.33333) H3A(0.33333) H3B(0.33333)
3.a Riding coordinates:
 O2(H2A,H2B), O3(H3A,H3B)
3.b Ternary CH refined with riding coordinates:
 C77(H77)
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)
;
_shelx_res_checksum              95276
_shelx_hkl_checksum              50443
_shelx_fab_checksum              68479
_olex2_submission_special_instructions 'No special instructions were received'