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_4077856
_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         'C39 H30  N4 P2 Ru, C H2 Cl2'
_chemical_formula_sum            'C40 H32 Cl2 N4 P2 Ru'
_chemical_formula_weight         802.61
_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_date             2007-06-19T02:04:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                82.087(4)
_cell_angle_beta                 89.623(4)
_cell_angle_gamma                75.665(4)
_cell_formula_units_Z            2
_cell_length_a                   11.7459(5)
_cell_length_b                   11.9723(5)
_cell_length_c                   13.2917(6)
_cell_measurement_reflns_used    7541
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.9495
_cell_measurement_theta_min      2.4946
_cell_volume                     1792.97(14)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_device_type
;
 Oxford Diffraction Xcalibur diffractometer
;
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_UB_11      0.0095657678
_diffrn_orient_matrix_UB_12      0.0201184259
_diffrn_orient_matrix_UB_13      0.0460873267
_diffrn_orient_matrix_UB_21      -0.0181392307
_diffrn_orient_matrix_UB_22      0.0582649041
_diffrn_orient_matrix_UB_23      -0.0242710889
_diffrn_orient_matrix_UB_31      -0.0588361292
_diffrn_orient_matrix_UB_32      0.0015990721
_diffrn_orient_matrix_UB_33      0.0134021908
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.116
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19495
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.93863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         9313
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.069
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0875
_reflns_number_gt                5735
_reflns_number_total             9313
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om2007503_si_001.cif
_cod_data_source_block           br1336
_cod_original_cell_volume        1792.97(13)
_cod_original_sg_symbol_Hall     -p_1
_cod_original_sg_symbol_H-M      P_-1
_cod_database_code               4077856