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_4134694
_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         'C106 H94 Mn4 N26 O18, 6(C5 N)'
_chemical_formula_sum            'C136 H94 Mn4 N32 O18'
_chemical_formula_weight         2684.19
_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   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                107.577(2)
_cell_angle_beta                 92.476(2)
_cell_angle_gamma                97.574(2)
_cell_formula_units_Z            1
_cell_length_a                   10.8346(4)
_cell_length_b                   16.7939(6)
_cell_length_c                   19.7458(7)
_cell_measurement_reflns_used    9159
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.27
_cell_volume                     3382.1(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      120.02
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0934
_diffrn_reflns_av_unetI/netI     0.0711
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            96194
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.581
_diffrn_reflns_theta_min         2.172
_exptl_absorpt_coefficient_mu    0.441
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0670 before and 0.0580 after correction.
The Ratio of minimum to maximum transmission is 0.9269.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             1378
_exptl_crystal_size_max          0.113
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.043
_refine_diff_density_max         2.440
_refine_diff_density_min         -1.212
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         15567
_refine_ls_number_restraints     400
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.1260
_refine_ls_R_factor_gt           0.0817
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2608
_refine_ls_wR_factor_ref         0.2928
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10345
_reflns_number_total             15567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01035_si_002.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 4134690--4134694.cif.'
_cod_database_code               4134694
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.952
_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, All O(H,H) groups
2. Rigid bond restraints
 N13, C47
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
C6 \\sim C5 \\sim C4 \\sim C7 \\sim C30 \\sim C27 \\sim C25 \\sim C24 \\sim C50
\\sim C26 \\sim C2 \\sim C17 \\sim C20 \\sim C28 \\sim C23 \\sim C49 \\sim C53
\\sim C8 \\sim C13 \\sim C14 \\sim C11 \\sim C21 \\sim C16 \\sim C1 \\sim C51
\\sim C15 \\sim C42 \\sim C19 \\sim C48 \\sim C3 \\sim C18 \\sim C29 \\sim C38
\\sim C52 \\sim C41 \\sim C9 \\sim C22 \\sim C31 \\sim C12 \\sim C40 \\sim C37
\\sim C10 \\sim C33 \\sim C36 \\sim C39 \\sim C35 \\sim C34 \\sim C32 \\sim C43
\\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C67 \\sim C68 \\sim C64 \\sim C65
\\sim C66 \\sim C57 \\sim C56 \\sim C55 \\sim C54 \\sim C58 \\sim C60 \\sim C61
\\sim C62 \\sim C63 \\sim C59: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C59) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C62)
\\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(C63) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C57) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C54)
\\sim Ueq, Uanis(N15) \\sim Ueq, Uanis(C58) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4.a Rotating group:
 O3(H3A,H3B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C24(H24), C26(H26), C49(H49), C16(H16), C51(H51), C15(H15),
 C42(H42), C19(H19), C48(H48), C18(H18), C38(H38), C52(H52), C41(H41), C40(H40),
  C37(H37), C33(H33), C36(H36), C39(H39), C35(H35), C34(H34), C43(H43),
 C44(H44), C45(H45), C46(H46), C47(H47)
4.c Fitted hexagon refined as free rotating group:
 C43(C44,C45,C46,C47,N13), C67(C68,C64,C65,C66,N16), C57(C56,C55,C54,N15,C58),
 C60(C61,C62,N14,C63,C59)
4.d Idealised Me refined as rotating group:
 C3(H3C,H3D,H3E), C29(H29A,H29B,H29C), C22(H22A,H22B,H22C), C12(H12A,H12B,
 H12C), C10(H10A,H10B,H10C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              37949
_shelx_hkl_checksum              58335
_shelx_fab_checksum              24003
_olex2_submission_special_instructions 'No special instructions were received'