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_4134691
_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
'C132 H108 Mn4 N28 O8, 8(C3 H7 N O), 2(C5 H5 N)'
_chemical_formula_sum            'C166 H174 Mn4 N38 O16'
_chemical_formula_weight         3177.18
_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
_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                 101.3080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.5195(7)
_cell_length_b                   47.357(2)
_cell_length_c                   14.8983(7)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.52
_cell_measurement_theta_min      2.21
_cell_volume                     10045.2(8)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       57
_diffrn_reflns_limit_k_min       -56
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            81002
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.424
_diffrn_reflns_theta_max         25.424
_diffrn_reflns_theta_min         2.207
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.306
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0602 before and 0.0483 after correction.
The Ratio of minimum to maximum transmission is 0.7859.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.050
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     998
_refine_ls_number_reflns         18260
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0793
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1495P)^2^+10.5123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2406
_refine_ls_wR_factor_ref         0.2541
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12786
_reflns_number_total             18260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01035_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4134690--4134694.cif.'
_cod_original_cell_volume        10045.3(8)
_cod_database_code               4134691
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C77-N17
 1.43 with sigma of 0.01
 C75-C77
 2.53 with sigma of 0.01
3. Rigid bond restraints
 C50, C51
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C50 \\sim C51: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C68) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C71)
\\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(N17) \\sim Ueq, Uanis(O6) \\sim Ueq,
Uanis(C77) \\sim Ueq, Uanis(C76) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5.a Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C42(H42A,H42B,H42C), C81(H81A,H81B,H81C),
 C83(H83A,H83B,H83C), C79(H79A,H79B,H79C), C69(H69A,H69B,H69C), C80(H80A,H80B,
 H80C), C68(H68A,H68B,H68C), C75(H75A,H75B,H75C), C77(H77A,H77B,H77C)
5.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C31(H31), C25(H25), C22(H22), C37(H37), C4(H4), C6(H6), C23(H23),
 C61(H61), C26(H26), C62(H62), C28(H28), C55(H55), C29(H29), C17(H17), C38(H38),
  C11(H11), C5(H5), C16(H16), C15(H15), C12(H12), C39(H39), C14(H14), C56(H56),
 C20(H20), C44(H44), C64(H64), C18(H18), C13(H13), C19(H19), C65(H65), C50(H50),
  C59(H59), C82(H82), C48(H48), C58(H58), C45(H45), C78(H78), C51(H51),
 C47(H47), C49(H49), C46(H46), C67(H67), C53(H53), C52(H52), C76(H76), C70(H70),
  C71(H71), C72(H72), C73(H73), C74(H74)
5.c Fitted hexagon refined as free rotating group:
 C70(C71,C72,N16,C73,C74)
5.d Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              28361
_shelx_hkl_checksum              97545
_olex2_submission_special_instructions 'No special instructions were received'