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_1571537
_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         'C69 H52 Br Cl2 N Os P3 S, C2 H4 Cl2, B F4'
_chemical_formula_sum            'C71 H56 B Br Cl4 F4 N Os P3 S'
_chemical_formula_weight         1546.85
_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             2023-03-12
_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                101.832(5)
_cell_angle_beta                 93.282(5)
_cell_angle_gamma                91.924(5)
_cell_formula_units_Z            2
_cell_length_a                   10.0004(13)
_cell_length_b                   11.4627(15)
_cell_length_c                   27.876(4)
_cell_measurement_reflns_used    9440
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      71.73
_cell_measurement_theta_min      3.94
_cell_volume                     3119.1(7)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.958
_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  0.0566
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            61603
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.391
_diffrn_reflns_theta_min         3.246
_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    7.694
_exptl_absorpt_correction_T_max  0.7535
_exptl_absorpt_correction_T_min  0.5138
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1502 before and 0.0808 after correction. The Ratio of minimum to maximum transmission is 0.6819. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic brownish orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       block
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.542
_refine_diff_density_min         -1.723
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         11830
_refine_ls_number_restraints     152
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0482P)^2^+11.0043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11449
_reflns_number_total             11830
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01993h2.cif
_cod_data_source_block           11d
_cod_depositor_comments
'Adding full bibliography for 1571535--1571544.cif.'
_cod_database_code               1571537
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.513
_shelx_estimated_absorpt_t_min   0.513
_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
 Cl2S-C2SB \\sim Cl3-C2SA
 with sigma of 0.02
 C1S-C2SB \\sim C1S-C2SA
 with sigma of 0.02
 Cl2S-C1S \\sim Cl3-C1S
 with sigma of 0.04
 Cl2S-C2SB \\sim Cl3-C2SA \\sim Cl1S-C1S
 with sigma of 0.02
 C2SA-C1S \\sim C2SB-C1S
 with sigma of 0.02
 F4-B02E \\sim F2A-B02E
 with sigma of 0.02
 F3-B02E \\sim F4A-B02E
 with sigma of 0.02
 F2-B02E \\sim F3A-B02E
 with sigma of 0.02
 F3-B02E \\sim F4A-B02E \\sim F4-B02E \\sim F2A-B02E \\sim F2-B02E \\sim
F3A-B02E \\sim F1-B02E
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1S \\sim Cl2S \\sim Cl3 \\sim C1S \\sim C2SA \\sim C2SB: within 2A with sigma
of 0.001 and sigma for terminal atoms of 0.002
F1 \\sim F2 \\sim F2A \\sim F3 \\sim F3A \\sim F4 \\sim F4A \\sim B02E: within
2A with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(Cl3)=Sof(H1Sc)=Sof(H1Sd)=Sof(C2SA)=Sof(H2Sc)=Sof(H2Sd)=1-FVAR(1)
 Sof(Cl2S)=Sof(H1Sa)=Sof(H1Sb)=Sof(C2SB)=Sof(H2Sa)=Sof(H2Sb)=FVAR(1)
 Sof(F2A)=Sof(F3A)=Sof(F4A)=1-FVAR(2)
 Sof(F2)=Sof(F3)=Sof(F4)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C1S(H1Sa,H1Sb), C1S(H1Sc,H1Sd), C2SA(H2Sc,H2Sd), C2SB(H2Sa,H2Sb)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C6(H6), C10(H10), C13(H13), C14(H14), 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), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69)
;
_shelx_res_checksum              91977
_olex2_submission_special_instructions 'No special instructions were received'