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_4072994
_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         'C26 H40 I3 P Ru'
_chemical_formula_sum            'C26 H40 I3 P Ru'
_chemical_formula_weight         865.32
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.267(2)
_cell_length_b                   17.974(2)
_cell_length_c                   18.631(3)
_cell_measurement_reflns_used    8129
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      23.28
_cell_measurement_theta_min      2.77
_cell_volume                     5782.3(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            64836
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    3.814
_exptl_absorpt_correction_T_max  0.3659
_exptl_absorpt_correction_T_min  0.2515
_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            brown
_exptl_crystal_density_diffrn    1.988
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.33
_refine_diff_density_max         1.190
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.288
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         7155
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.288
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0073P)^2^+40.7845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0828
_reflns_number_gt                6344
_reflns_number_total             7155
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om061192vsi20061231_072132.cif
_cod_data_source_block           sc456
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        5782.3(14)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4072994