Reactions of Isocyanides with Metal Carbyne Complexes: Isolation and Characterization of Metallacyclopropenimine Intermediates.
Luo, Ming; Long, Lipeng; Zhang, Hong; Yang, Yuhui; Hua, Yuhui; Liu, Gang; Lin, Zhenyang; Xia, Haiping; Journal of the American Chemical Society 139 (2017) 1822–1825; doi:10.1021/jacs.6b13275

data_4125696
_publ_section_title
;
 Reactions of Isocyanides with Metal Carbyne Complexes: Isolation and
 Characterization of Metallacyclopropenimine Intermediates.
;
_journal_issue                   5
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1822
_journal_page_last               1825
_journal_paper_doi               10.1021/jacs.6b13275
_journal_volume                  139
_journal_year                    2017
_chemical_formula_sum            'C67 H73 Cl4 N3 O3 Os P2'
_chemical_formula_weight         1362.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.498(2)
_cell_angle_beta                 98.272(2)
_cell_angle_gamma                108.058(3)
_cell_formula_units_Z            2
_cell_length_a                   11.6666(4)
_cell_length_b                   12.6271(4)
_cell_length_c                   22.2623(6)
_cell_measurement_reflns_used    15792
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.9909
_cell_measurement_theta_min      2.6576
_cell_volume                     3066.10(18)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33106
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    2.355
_exptl_absorpt_correction_T_max  0.5905
_exptl_absorpt_correction_T_min  0.4379
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.566
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         10768
_refine_ls_number_restraints     1638
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+5.7449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0936
_reflns_number_gt                9578
_reflns_number_total             10768
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b13275_si_002.cif
_cod_data_source_block           4c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        3066.09(17)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4125696