New d4 dihydrides of Ru(iv) and Os(iv) with ?-donor ligands: M(H)2(chelate)(PiPr3)2 with chelate =ortho-XYC6H4 with X, Y = O, NR; R = H or CH3
Ferrando-Miguel, German; Wu, Peng; Huffman, John C.; Caulton, Kenneth G.; New Journal of Chemistry 29 (2005) 193–; doi:10.1039/b411487f

data_7052415
_publ_section_title
;
 New d4 dihydrides of Ru(iv) and Os(iv) with ?-donor ligands:
 M(H)2(chelate)(PiPr3)2 with chelate =ortho-XYC6H4 with X, Y = O, NR; R
 = H or CH3
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              193
_journal_paper_doi               10.1039/b411487f
_journal_volume                  29
_journal_year                    2005
_chemical_formula_sum            'C25 H52 N2 Os P2'
_chemical_formula_weight         632.83
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 97.4220(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9882(3)
_cell_length_b                   21.8475(9)
_cell_length_c                   14.1438(6)
_cell_measurement_reflns_used    7153
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.36
_cell_volume                     2754.14(19)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local package)'
_computing_molecular_graphics    'XMView; WMView; (local package)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
'   0.30 degree frames measured for  30.16 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       '\w 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  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22120
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  640
_diffrn_standards_number         7154
_exptl_absorpt_coefficient_mu    4.761
_exptl_absorpt_correction_T_max  0.7019
_exptl_absorpt_correction_T_min  0.3293
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.797
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.265(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         12431
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0698
_reflns_number_gt                11366
_reflns_number_total             12431
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b411487f.txt
_cod_data_source_block           01088
_cod_database_code               7052415