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_1565817
_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         '2(C76 H76 N8 Pd2)'
_chemical_formula_sum            'C152 H152 N16 Pd4'
_chemical_formula_weight         2628.49
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-27 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                68.5900(10)
_cell_angle_beta                 89.019(2)
_cell_angle_gamma                82.809(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6940(4)
_cell_length_b                   20.7153(6)
_cell_length_c                   27.7180(9)
_cell_measurement_reflns_used    9697
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      66.65
_cell_measurement_theta_min      2.31
_cell_volume                     6199.0(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            132146
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.791
_diffrn_reflns_theta_max         66.791
_diffrn_reflns_theta_min         1.713
_exptl_absorpt_coefficient_mu    5.076
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1102 before and 0.0543 after correction.
The Ratio of minimum to maximum transmission is 0.7163.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brownish
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       needle
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.009
_refine_diff_density_min         -1.740
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1593
_refine_ls_number_reflns         21927
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0852P)^2^+11.5892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1471
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19321
_reflns_number_total             21927
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06514a2.cif
_cod_data_source_block           cu_20210511a_0m_a_sq
_cod_depositor_comments
'Adding full bibliography for 1565814--1565817.cif.'
_cod_database_code               1565817
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.863
_shelx_estimated_absorpt_t_min   0.605
_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. Restrained distances
 C52-C51 = C82-C81
 1.54 with sigma of 0.01
 C81-C49 = C51-C49
 1.51 with sigma of 0.01
 H4A_$1-H4A
 2.2 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C51 \\sim C52 \\sim C81 \\sim C82: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 1.7A
Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C82)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=1-FVAR(1)
 Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C02E(H02A,H02B), C5(H5A,H5B), C7(H7A,H7B), C14(H14A,H14B), C23(H23A,H23B),
 C25(H25A,H25B), C43(H43A,H43B), C45(H45A,H45B), C51(H51A,H51B), C53(H53A,H53B),
  C61(H61A,H61B), C63(H63A,H63B), C5A(H5AA,H5AB), C7A(H7AA,H7AB), C8(H8B,H8C),
 C14A(H14C,H14D), C23A(H23C,H23D), C25A(H25C,H25D), C43A(H43C,H43D), C45A(H45C,
 H45D), C51A(H51C,H51D), C53A(H53C,H53D), C61A(H61C,H61D), C63A(H63C,H63D),
 C81(H81A,H81B)
5.b Aromatic/amide H refined with riding coordinates:
 N4(H4), N8(H8), C9(H9), C18(H18), C28(H28), C29(H29), C32(H32), C35(H35),
 C38(H38), C47(H47), C56(H56), C66(H66), C67(H67), C70(H70), C73(H73), C76(H76),
  N4A(H4A), N8A(H8A), C9A(H9A), C18A(H18A), C28A(H28A), C29A(H29A), C32A(H32A),
 C35A(H35A), C38A(H38A), C47A(H47A), C56A(H56A), C66A(H66A), C67A(H67A),
 C70A(H70A), C73A(H73A), C76A(H76A)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C44(H44A,H44B,H44C), C46(H46A,
 H46B,H46C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C62(H62A,H62B,H62C),
 C64(H64A,H64B,H64C), C6A(H6AA,H6AB,H6AC), C8A(H8AA,H8AB,H8AC), C15A(H15D,H15E,
 H15F), C17A(H17D,H17E,H17F), C24A(H24D,H24E,H24F), C26A(H26D,H26E,H26F),
 C44A(H44D,H44E,H44F), C46A(H46D,H46E,H46F), C52A(H52D,H52E,H52F), C54A(H54D,
 H54E,H54F), C62A(H62D,H62E,H62F), C64A(H64D,H64E,H64F), C82(H82A,H82B,H82C)
;
_shelx_res_checksum              1467
_shelx_hkl_checksum              13666
_shelx_fab_checksum              30925
_olex2_submission_special_instructions 'No special instructions were received'