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_1571540
_publ_section_title
;
 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         'C63 H50 Cl2 N Os P3, 2(Cl)'
_chemical_formula_sum            'C63 H50 Cl4 N Os P3'
_chemical_formula_weight         1245.95
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-12-17 deposited with the CCDC.	2024-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.8120(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5847(5)
_cell_length_b                   20.8470(8)
_cell_length_c                   21.1394(8)
_cell_measurement_reflns_used    9617
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      72.32
_cell_measurement_theta_min      4.11
_cell_volume                     5533.7(4)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_collection       'Apex3 (Bruker 2018)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            95746
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.322
_diffrn_reflns_theta_min         2.980
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.262
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5146
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1144 before and 0.0571 after correction. The Ratio of minimum to maximum transmission is 0.6829. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic yellowish orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       block
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.640
_refine_diff_density_min         -1.743
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         10922
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0371P)^2^+18.7166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0830
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10625
_reflns_number_total             10922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01993h2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 1571535--1571544.cif.'
_cod_database_code               1571540
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: Cl2S(0.5) Cl3S(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C6(H6), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23),
  C24(H24), C25(H25), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31),
 C32(H32), C33(H33), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C41(H41),
  C42(H42), C43(H43), C44(H44), C45(H45), C47(H47), C48(H48), C49(H49),
 C50(H50), C51(H51), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C59(H59),
  C60(H60), C61(H61), C62(H62), C63(H63)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              43068
_shelx_fab_checksum              44161
_olex2_submission_special_instructions 'No special instructions were received'