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_1571536
_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 H49 Cl2 N Os P3, C2 H4 Cl2, B F4'
_chemical_formula_sum            'C65 H53 B Cl4 F4 N Os P3'
_chemical_formula_weight         1359.80
_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             2023-03-04
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2023-12-17 deposited with the CCDC.	2024-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.337(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.014(3)
_cell_length_b                   21.683(3)
_cell_length_c                   12.1814(15)
_cell_measurement_reflns_used    9029
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      72.43
_cell_measurement_theta_min      4.08
_cell_volume                     5753.1(13)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 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     1.54178
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            54624
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.417
_diffrn_reflns_theta_min         4.078
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.11
_diffrn_source_power             0.05550000000000001
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.140
_exptl_absorpt_correction_T_max  0.7535
_exptl_absorpt_correction_T_min  0.4303
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1767 before and 0.0872 after correction.
The Ratio of minimum to maximum transmission is 0.5711.
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    1.570
_exptl_crystal_description       block
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.485
_refine_diff_density_min         -1.293
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         10943
_refine_ls_number_restraints     159
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+18.0121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9704
_reflns_number_total             10943
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01993h2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 1571535--1571544.cif.'
_cod_original_cell_volume        5752.9(12)
_cod_database_code               1571536
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.535
_shelx_estimated_absorpt_t_min   0.535
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 F4-B01V \\sim F4A-B01V
 with sigma of 0.02
 F2-B01V \\sim F2A-B01V
 with sigma of 0.02
 B01V-F3 \\sim B01V-F3A
 with sigma of 0.02
 F3A-B01V \\sim F3-B01V \\sim C20-C19 \\sim F2-B01V \\sim F2A-B01V \\sim
F1-B01V \\sim F4A-B01V \\sim F4-
 B01V
 with sigma of 0.02
 Cl2S-C2SA \\sim Cl3S-C2SB
 with sigma of 0.02
 C1S-C2SA \\sim C1S-C2SB
 with sigma of 0.02
 Cl2S-C1S \\sim Cl3S-C1S
 with sigma of 0.04
 C2SB-C1S \\sim C2SA-C1S
 with sigma of 0.02
 Cl1S-C1S \\sim Cl2S-C2SA \\sim Cl3S-C2SB
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F1 \\sim B01V \\sim F2 \\sim F3 \\sim F4 \\sim F2A \\sim F3A \\sim F4A: within
2A with sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Cl1S \\sim C1S \\sim Cl2S \\sim C2SA \\sim Cl3S \\sim C2SB: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
4. Others
 Sof(F2A)=Sof(F3A)=Sof(F4A)=1-FVAR(1)
 Sof(F2)=Sof(F3)=Sof(F4)=FVAR(1)
 Sof(H1SC)=Sof(H1SD)=Sof(Cl3S)=Sof(C2SB)=Sof(H2SC)=Sof(H2SD)=1-FVAR(2)
 Sof(H1SA)=Sof(H1SB)=Sof(Cl2S)=Sof(C2SA)=Sof(H2SA)=Sof(H2SB)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C1S(H1SC,H1SD), C1S(H1SA,H1SB), C2SA(H2SA,H2SB), C2SB(H2SC,H2SD)
5.b Aromatic/amide H refined with riding coordinates:
 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)
;
_shelx_res_checksum              21313
_olex2_submission_special_instructions 'No special instructions were received'