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_4134690
_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 H84 Mn4 N20 O16, 6(C H4 O)'
_chemical_formula_sum            'C82 H108 Mn4 N20 O22'
_chemical_formula_weight         1945.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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                 90.5243(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.66791(14)
_cell_length_b                   35.5294(6)
_cell_length_c                   18.9331(3)
_cell_measurement_reflns_used    9719
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.2440
_cell_measurement_theta_min      4.3900
_cell_volume                     5157.85(15)
_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    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22060
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.099
_diffrn_reflns_theta_min         4.404
_exptl_absorpt_coefficient_mu    4.498
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39708
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.864
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         10194
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0906P)^2^+3.0294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1488
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9113
_reflns_number_total             10194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01035_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4134690--4134694.cif.'
_cod_original_cell_volume        5157.84(16)
_cod_database_code               4134690
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.346
_shelx_estimated_absorpt_t_min   0.191
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 O7(H7), O8(H8), O4(H4), O3(H3), O10(H10), O11(H11), O9(H9)
2.b Me refined with riding coordinates:
 C3(H3A,H3B,H3C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C29(H29A,H29B,
 H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7A), C15(H15), C16(H16), C18(H18), C19(H19), C24(H24),
 C25(H25), C26(H26), C34(H34), C35(H35), C37(H37), C38(H38)
2.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C22(H22A,H22B,H22C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              74217
_shelx_hkl_checksum              84916
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20