Isomerization reactions of metal vinylidene units.
Zheng, Xuejuan; Huang, Fanping; Li, Xinyuan; Zhuo, Kaiyue; Chen, Dafa; Luo, Ming; Xia, Haiping; Chemical science 15 (2024) 8443–8450; doi:10.1039/d4sc01993h

data_1571541
_publ_section_title
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 Isomerization reactions of metal vinylidene units.
;
_journal_issue                   22
_journal_name_full               'Chemical science'
_journal_page_first              8443
_journal_page_last               8450
_journal_paper_doi               10.1039/d4sc01993h
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C64 H50 Cl N O Os P3, 3(C H2 Cl2), C24 H20 B'
_chemical_formula_sum            'C91 H76 B Cl7 N O Os P3'
_chemical_formula_weight         1741.59
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-16
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-12-17 deposited with the CCDC.	2024-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                78.0980(10)
_cell_angle_beta                 81.6520(10)
_cell_angle_gamma                70.8870(10)
_cell_formula_units_Z            2
_cell_length_a                   14.0545(4)
_cell_length_b                   17.0441(5)
_cell_length_c                   17.7828(6)
_cell_measurement_reflns_used    9610
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      72.13
_cell_measurement_theta_min      4.37
_cell_volume                     3924.5(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'Apex3 (Bruker 2018)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2014'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Bruker PHOTON II area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker CMOS area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            76359
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.146
_diffrn_reflns_theta_min         2.784
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.221
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.4050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1436 before and 0.0854 after correction.
The Ratio of minimum to maximum transmission is 0.5374.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic orangish orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       block
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.933
_refine_diff_density_min         -1.634
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     946
_refine_ls_number_reflns         15401
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0521P)^2^+8.2818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.0958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15355
_reflns_number_total             15401
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01993h2.cif
_cod_data_source_block           Int1'
_cod_depositor_comments
'Adding full bibliography for 1571535--1571544.cif.'
_cod_database_code               1571541
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.455
_shelx_estimated_absorpt_t_min   0.369
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C6(H6), C12(H12), C13(H13), C14(H14), C15(H15),
 C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
  C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33),
 C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43),
  C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51),
 C52(H52), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C60(H60), C61(H61),
  C62(H62), C63(H63), C64(H64), C66(H66), C67(H67), C68(H68), C69(H69),
 C70(H70), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C78(H78), C79(H79),
  C80(H80), C81(H81), C82(H82), C84(H84), C85(H85), C86(H86), C87(H87), C88(H88)
3.c :
 C9(H9)
;
_shelx_res_checksum              3973
_olex2_submission_special_instructions 'No special instructions were received'