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_7052414
_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            'C30 H54 O2 P2 Ru'
_chemical_formula_weight         609.775
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method
'minor manual editing of SDT2CIF v. 1.2 BETA  output'
_cell_angle_alpha                77.529(5)
_cell_angle_beta                 89.453(5)
_cell_angle_gamma                76.548(5)
_cell_formula_units_Z            2
_cell_length_a                   11.224(2)
_cell_length_b                   11.907(2)
_cell_length_c                   12.510(2)
_cell_measurement_reflns_used    952
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      3.09
_cell_volume                     1586.2(5)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local package)'
_computing_molecular_graphics    'XTEL, local package'
_computing_publication_material  'XTEL, local package'
_computing_structure_refinement  'XTEL, local package'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_details
'   0.30 degree frames measured for   5.15 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_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  2810
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3
_diffrn_reflns_theta_full        23.2683
_diffrn_reflns_theta_max         23.2683
_diffrn_reflns_theta_min         2.17107
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  208
_diffrn_standards_number         953
_exptl_absorpt_coefficient_mu    0.6186
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             648
_exptl_crystal_size_max          .45
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .25
_refine_diff_density_max         0.88
_refine_diff_density_min         -0.99
_refine_ls_abs_structure_details none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0330
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         2810
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.0044
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w^-1^=\s^2^(F)+(.00F)^2^
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0346
_reflns_number_gt                2810
_reflns_number_total             3450
_reflns_threshold_expression     'Fo^2^> 2.33\s(Fo^2^)'
_cod_data_source_file            b411487f.txt
_cod_data_source_block           MSC01012
_cod_original_cell_volume        1586.1(5)
_cod_original_formula_sum        'C30 H54 O2 P2 Ru1'
_cod_database_code               7052414