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_4125693
_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_moiety         'C68 H60 Cl N O2 Os P3, F6 P'
_chemical_formula_sum            'C68 H60 Cl F6 N O2 Os P4'
_chemical_formula_weight         1386.70
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-08-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                94.495(2)
_cell_angle_beta                 94.496(2)
_cell_angle_gamma                101.582(3)
_cell_formula_units_Z            2
_cell_length_a                   13.3911(4)
_cell_length_b                   14.4040(5)
_cell_length_c                   17.5220(5)
_cell_measurement_reflns_used    10751
_cell_measurement_temperature    172.95(10)
_cell_measurement_theta_max      26.3370
_cell_measurement_theta_min      3.7040
_cell_volume                     3285.37(18)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_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    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      172.95(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24766
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.99
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.139
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89502
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.912
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         11529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+4.9478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0707
_reflns_number_gt                10819
_reflns_number_total             11529
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b13275_si_002.cif
_cod_data_source_block           2
_cod_database_code               4125693
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Me refined with riding coordinates:
 C64(H64A,H64B,H64C), C75(H75A,H75B,H75C), C77(H77A,H77B,H77C), C9(H9A,H9B,H9C)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7A), C201(H20A), C13(H13A), C20(H20B), C3(H3A), C24(H24A), C25(H25A),
 C26(H26A), C27(H27A), C28(H28A), C5(H5A), C35(H35A), C36(H36A), C37(H37A),
 C38(H38A), C39(H39A), C40(H40A), C41(H41A), C43(H43A), C45(H45A), C46(H46A),
 C47(H47A), C48(H48A), C49(H49A), C50(H50A), C52(H52A), C53(H53A), C54(H54A),
 C56(H56A), C57(H57A), C58(H58A), C59(H59A), C60(H60A), C61(H61A), C62(H62A),
 C63(H63A), C65(H65A), C67(H67A), C68(H68A), C69(H69A), C70(H70A), C71(H71A),
 C72(H72A), C76(H76A), C79(H79A), C80(H80A), C81(H81A), C82(H82A)
;
_olex2_submission_special_instructions 'No special instructions were received'