Substitution of Tetracyanoethene by Ethynyl‒Metal Complexes Gives Tricyanovinylethynyl (Tricyanobutenynyl) Derivatives: Syntheses, Protonation, and Addition of Metal‒Ligand Fragments
Bruce, Michael I.; Fox, Mark A.; Low, Paul J.; Nicholson, Brian K.; Parker, Christian R.; Patalinghug, Wyona C.; Skelton, Brian W.; White, Allan H.; Organometallics 31 (2012) 2639–; doi:10.1021/om2007503

data_4077855
_publ_section_title
;
 Substitution of Tetracyanoethene by Ethynyl--Metal Complexes Gives
 Tricyanovinylethynyl (Tricyanobutenynyl) Derivatives: Syntheses,
 Protonation, and Addition of Metal--Ligand Fragments
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2639
_journal_paper_doi               10.1021/om2007503
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C79 H78 N3 Os P4 Ru, F6 P'
_chemical_formula_sum            'C79 H78 F6 N3 Os P5 Ru'
_chemical_formula_weight         1629.56
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2006-12-14T19:36:29-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 100.138(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9050(10)
_cell_length_b                   14.7607(8)
_cell_length_c                   23.7010(10)
_cell_measurement_reflns_used    10230
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.789
_cell_measurement_theta_min      2.3928
_cell_volume                     7199.3(6)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
        (compiled Aug 28 2006,13:05:05)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
        (compiled Aug 28 2006,13:05:05)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
        (compiled Aug 28 2006,13:05:05)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type
;
 Oxford Diffraction Xcalibur diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0175491947
_diffrn_orient_matrix_UB_12      -0.0384970678
_diffrn_orient_matrix_UB_13      0.006639106
_diffrn_orient_matrix_UB_21      0.0290790377
_diffrn_orient_matrix_UB_22      -0.0189430465
_diffrn_orient_matrix_UB_23      0.0153550202
_diffrn_orient_matrix_UB_31      -0.0058610976
_diffrn_orient_matrix_UB_32      0.0214942703
_diffrn_orient_matrix_UB_33      0.0253720174
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_unetI/netI     0.1736
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            51366
_diffrn_reflns_theta_full        30.
_diffrn_reflns_theta_max         30.98
_diffrn_reflns_theta_min         2.4
_exptl_absorpt_coefficient_mu    2.145
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.81168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
        (compiled Aug 28 2006,13:05:05)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3284
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.113
_refine_diff_density_min         -2.242
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         10772
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.1392
_refine_ls_R_factor_gt           0.0749
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0748P)^2^+42.5534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.191
_refine_ls_wR_factor_ref         0.2044
_reflns_number_gt                5503
_reflns_number_total             10772
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om2007503_si_001.cif
_cod_data_source_block           br1298
_cod_original_sg_symbol_Hall     -c_2yc
_cod_database_code               4077855