Synthesis, Structure, and Reactivity of Four-, Five-, and Six-Coordinate Ruthenium Carbyne Complexes
Caskey, Stephen R.; Stewart, Michael H.; Ahn, Yi Joon; Johnson, Marc J. A.; Rowsell, Jesse L. C.; Kampf, Jeff W.; Organometallics 26 (2007) 1912–; doi:10.1021/om061192v

data_4072996
_publ_section_title
;
 Synthesis, Structure, and Reactivity of Four-, Five-, and Six-Coordinate
 Ruthenium Carbyne Complexes
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1912
_journal_paper_doi               10.1021/om061192v
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         '2(C44 H73 Cl2 P2 Ru), 5(C H2 Cl2), 2(B F4)'
_chemical_formula_sum            'C93 H156 B2 Cl14 F8 P4 Ru2'
_chemical_formula_weight         2270.12
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.152(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.626(4)
_cell_length_b                   32.847(12)
_cell_length_c                   28.253(10)
_cell_measurement_reflns_used    2048
_cell_measurement_temperature    108(2)
_cell_measurement_theta_max      29.54
_cell_measurement_theta_min      2.28
_cell_volume                     10652(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART-1K'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      108(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART 1K'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            229661
_diffrn_reflns_theta_full        29.59
_diffrn_reflns_theta_max         29.59
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_T_max  0.8172
_exptl_absorpt_correction_T_min  0.7334
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Blessing, R. Acta Cryst. (1995) A51 33-38.
  Sheldrick, G.  SADABS (Version 2.10) Bruker/Siemens area
  detector absorption and other corrections, University of 
  Gottingen, Germany 2003.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4728
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.479
_refine_diff_density_min         -1.534
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1110
_refine_ls_number_reflns         29746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+46.8976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1431
_reflns_number_gt                22201
_reflns_number_total             29746
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om061192vsi20061231_072132.cif
_cod_data_source_block           sc1488a
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4072996