Ru and Os Complexes Containing a P,N-Donor Heterotopic Ligand: The Effect of Solvent on Stereochemistry
Dabb, Serin L.; Messerle, Barbara A.; Smith, Matthew K.; Willis, Anthony C.; Inorganic Chemistry 47 (2008) 3034–3044; doi:10.1021/ic7019044

data_4304396
_publ_section_title
;
 Ru and Os Complexes Containing a P,N-Donor Heterotopic Ligand:
 The Effect of Solvent on Stereochemistry
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3034
_journal_page_last               3044
_journal_paper_doi               10.1021/ic7019044
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C35 H36 Cl4 N4 Os P2'
_chemical_formula_weight         906.62
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 92.48(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.250(2)
_cell_length_b                   19.019(4)
_cell_length_c                   37.938(8)
_cell_measurement_reflns_used    493000
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.91
_cell_volume                     7389(3)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        'X -Seed'
_computing_molecular_graphics    'X-Seed / POV-Ray'
_computing_publication_material  'Microsoft Office 2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       ' \f and \w scans with CCD '
_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  0.0692
_diffrn_reflns_av_sigmaI/netI    0.0611
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            62906
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.858
_exptl_absorpt_correction_T_max  0.739
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.434
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.230
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         12347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.230
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+72.5806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1254
_reflns_number_gt                9152
_reflns_number_total             12347
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7019044-file002.cif
_cod_data_source_block           c:new10
_cod_database_code               4304396