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_4077858
_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         'C84 H74 N3 P4 Ru2, F6 P'
_chemical_formula_sum            'C84 H74 F6 N3 P5 Ru2'
_chemical_formula_weight         1596.45
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2008-10-14T14:31:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   36.723(17)
_cell_length_b                   68.84(3)
_cell_length_c                   11.415(5)
_cell_measurement_reflns_used    6848
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      2.22
_cell_volume                     28857(2)
_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 0.995
_diffrn_measured_fraction_theta_max 0.988
_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  .072
_diffrn_reflns_av_unetI/netI     0.1085
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       89
_diffrn_reflns_limit_k_min       -89
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            47047
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.66
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  .94
_exptl_absorpt_correction_T_min  .80
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    1.47
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             13056
_exptl_crystal_size_max          .6
_exptl_crystal_size_mid          .12
_exptl_crystal_size_min          .1
_refine_diff_density_max         0.825
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     906
_refine_ls_number_reflns         15861
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.062
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+242.9883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1575
_reflns_number_gt                10929
_reflns_number_total             15861
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om2007503_si_001.cif
_cod_data_source_block           br1209
_cod_original_cell_volume        28857(22)
_cod_original_sg_symbol_Hall     f_2_-2d
_cod_original_sg_symbol_H-M      F_d_d_2
_cod_database_code               4077858