Subcomponent Self-Assembly of Covalent Metallacycles Templated by Catalytically Active Seven-Coordinate Transition Metal Centers.
Li, Zhi-Wei; Wang, Xin; Wei, Lian-Qiang; Ivanović-Burmazović, Ivana; Liu, Gao-Feng; Journal of the American Chemical Society 142 (2020) 7283–7288; doi:10.1021/jacs.0c01035

data_4134692
_publ_section_title
;
 Subcomponent Self-Assembly of Covalent Metallacycles Templated by
 Catalytically Active Seven-Coordinate Transition Metal Centers.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7283
_journal_page_last               7288
_journal_paper_doi               10.1021/jacs.0c01035
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety
'C76 H72 Co4 N24 O12, 6(Cl O4), 2(C H4 O), 2(C6 H6)'
_chemical_formula_sum            'C90 H84 Cl6 Co4 N24 O38'
_chemical_formula_weight         2558.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-08-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 123.828(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   47.019(2)
_cell_length_b                   8.0598(3)
_cell_length_c                   41.8518(19)
_cell_measurement_reflns_used    7383
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      62.5790
_cell_measurement_theta_min      3.7500
_cell_volume                     13175.4(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_av_unetI/netI     0.1003
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            34165
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        65.484
_diffrn_reflns_theta_max         65.484
_diffrn_reflns_theta_min         3.760
_exptl_absorpt_coefficient_mu    5.674
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       block
_exptl_crystal_F_000             5224
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.136
_refine_diff_density_min         -1.052
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     684
_refine_ls_number_reflns         11078
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.233
_refine_ls_R_factor_all          0.1740
_refine_ls_R_factor_gt           0.1293
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3523
_refine_ls_wR_factor_ref         0.3894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6347
_reflns_number_total             11078
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01035_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4134690--4134694.cif.'
_cod_original_cell_volume        13175.2(11)
_cod_database_code               4134692
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C35, C36
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
C35 \\sim C36: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C45) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O16) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4.a Riding coordinates:
 O3(H3A,H3B), O6(H6A,H6B), O19(H19A)
4.b Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C26(H26A,H26B,H26C), C34(H34A,H34B,H34C),
 C36(H36A,H36B,H36C)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C12(H12), C15(H15), C16(H16), C18(H18), C19(H19),
 C21(H21), C22(H22), C24(H24), C29(H29), C30(H30), C31(H31), C39(H39), C40(H40),
  C41(H41), C42(H42), C43(H43), C44(H44)
4.d Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C7,N3), C14(C15,C16,C17,C18,C19), C28(C29,C30,C31,C32,N9),
 C39(C40,C41,C42,C43,C44)
4.e Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              95876
_shelx_hkl_checksum              7227
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20