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_4125695
_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            'C70.4 H62.8 B Cl1.8 F4 N O2 Os P3'
_chemical_formula_weight         1388.55
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.662(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.7295(5)
_cell_length_b                   13.9429(2)
_cell_length_c                   20.7926(4)
_cell_measurement_reflns_used    9132
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      62.2070
_cell_measurement_theta_min      3.8790
_cell_volume                     6517.7(2)
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0571
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32935
_diffrn_reflns_theta_full        62.14
_diffrn_reflns_theta_max         62.14
_diffrn_reflns_theta_min         3.73
_exptl_absorpt_coefficient_mu    5.527
_exptl_absorpt_correction_T_max  0.5568
_exptl_absorpt_correction_T_min  0.3899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   empirical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2803
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.788
_refine_diff_density_min         -1.375
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         10263
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0701
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1275P)^2^+41.4953P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2051
_refine_ls_wR_factor_ref         0.2167
_reflns_number_gt                8767
_reflns_number_total             10263
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b13275_si_002.cif
_cod_data_source_block           3c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C70.40 H62.80 B Cl1.80 F4 N O2 Os P3'
_cod_database_code               4125695