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_4077854
_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         'C48 H35 N3 P2 Ru'
_chemical_formula_sum            'C48 H35 N3 P2 Ru'
_chemical_formula_weight         816.8
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2008-10-14T10:12:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 100.1350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4978(7)
_cell_length_b                   17.5630(9)
_cell_length_c                   19.6050(10)
_cell_measurement_reflns_used    7760
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      37.88
_cell_measurement_theta_min      2.41
_cell_volume                     3897.2(4)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'xtal ADDREF SORTRF'
_computing_molecular_graphics    xtal
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.97
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  .022
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            81052
_diffrn_reflns_theta_full        37.5
_diffrn_reflns_theta_max         37.88
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  .83
_exptl_absorpt_correction_T_min  .684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          .45
_exptl_crystal_size_mid          .38
_exptl_crystal_size_min          .35
_refine_diff_density_max         0.903
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.07
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         20404
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+1.4120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.075
_reflns_number_gt                17661
_reflns_number_total             20404
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om2007503_si_001.cif
_cod_data_source_block           br1260
_cod_original_sg_symbol_Hall     -p_2yn
_cod_original_sg_symbol_H-M      P_1_21/n_1
_cod_database_code               4077854