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_4134693
_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         'C37 H34 F3 N10 O10 S Zn2'
_chemical_formula_sum            'C37 H34 F3 N10 O10 S Zn2'
_chemical_formula_weight         998.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 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                 115.880(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8683(17)
_cell_length_b                   35.964(4)
_cell_length_c                   15.7673(18)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.18
_cell_measurement_theta_min      2.66
_cell_volume                     7585.6(15)
_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      119.99
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_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  0.1014
_diffrn_reflns_av_unetI/netI     0.1533
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            62698
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.589
_diffrn_reflns_theta_min         1.522
_exptl_absorpt_coefficient_mu    0.705
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.874
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2036
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.702
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.329
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         17661
_refine_ls_number_restraints     152
_refine_ls_restrained_S_all      1.340
_refine_ls_R_factor_all          0.2173
_refine_ls_R_factor_gt           0.1471
_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^)+(0.2200P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4230
_refine_ls_wR_factor_ref         0.4519
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8662
_reflns_number_total             17661
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01035_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 4134690--4134694.cif.'
_cod_database_code               4134693
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.902
_shelx_estimated_absorpt_t_min   0.869
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Zn3-O11
 2.11 with sigma of 0.01
 C21-C22
 1.38 with sigma of 0.01
 C23-C22
 1.39 with sigma of 0.01
 O3-C36
 1.32 with sigma of 0.01
 C26-C27
 1.35 with sigma of 0.01
 C28-C27
 1.42 with sigma of 0.01
3. Rigid bond restraints
 N4, N5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Zn2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N5, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N5 \\sim N4: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C38 \\sim O10: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C23 \\sim C22: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
O11 \\sim C38: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C9 \\sim C10: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
N5 \\sim C11: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
Zn3 \\sim O11: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
Zn2: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N6) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C9) \\sim
Ueq, Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq, Uanis(N5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C32) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C21)
\\sim Ueq, Uanis(N8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Zn3) \\sim Ueq, Uanis(O11) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N5) = Uanis(O2)
Uanis(O7) = Uanis(O9)
5. Others
 Fixed Sof: H9A(0.5) H9B(0.5)
6.a Riding coordinates:
 O9(H9A,H9B)
6.b Me refined with riding coordinates:
 C28(H28A,H28B,H28C), C36(H36A,H36B,H36C)
6.c Aromatic/amide H refined with riding coordinates:
 N5(H5), N1(H1), N11(H11), C17(H17), C16(H16), C14(H14), C13(H13), C5(H5A),
 C6(H6), C7(H7), C32(H32), C31(H31), C35(H35), C34(H34), C25(H25), C24(H24),
 N6(H6A), C22(H22), C23(H23)
6.d Fitted hexagon refined as free rotating group:
 C12(C17,C16,C15,C14,C13), C8(N3,C4,C5,C6,C7), C33(C32,C31,C30,C35,C34)
6.e Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C10(H10A,H10B,H10C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              65482
_shelx_hkl_checksum              30972
_shelx_fab_checksum              17056
_olex2_submission_special_instructions 'No special instructions were received'