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_4077853
_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         'C38 H29 N3 P2 Ru'
_chemical_formula_sum            'C38 H29 N3 P2 Ru'
_chemical_formula_weight         690.65
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2008-10-14T12:10:37-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.4332(16)
_cell_length_b                   16.4391(12)
_cell_length_c                   17.9893(14)
_cell_measurement_reflns_used    6131
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.49
_cell_measurement_theta_min      2.21
_cell_volume                     6338.4(8)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        xtal
_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 0.996
_diffrn_measured_fraction_theta_max 0.971
_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  .054
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            89975
_diffrn_reflns_theta_full        33
_diffrn_reflns_theta_max         33.64
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_T_max  .94
_exptl_absorpt_correction_T_min  .79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          .48
_exptl_crystal_size_mid          .16
_exptl_crystal_size_min          .1
_refine_diff_density_max         2.12
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         23867
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.048
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+5.3949P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1165
_reflns_number_gt                17574
_reflns_number_total             23867
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om2007503_si_001.cif
_cod_data_source_block           br1221
_cod_original_sg_symbol_Hall     p_2c_-2ac
_cod_original_sg_symbol_H-M      P_c_a_21
_cod_database_code               4077853