Effect of Lewis Acidity on the Synthesis of RuHCl(CO)(phosphine)2: Subtle Influence of Steric and Electronic Effects among PiPr3, PiPr2(3,5-(CF3)2C6H3), and PiPr2Me
Alexei V. Marchenko; John C. Huffman; Pedro Valerga; Manuel Jiménez Tenorio; M Carmen Puerta; Kenneth G. Caulton; Inorganic Chemistry 40 (2001) 6444–6450; doi:10.1021/ic000500t

data_4320624
_publ_section_title
;
 Effect of Lewis Acidity on the Synthesis of RuHCl(CO)(phosphine)2: Subtle
 Influence of Steric and Electronic Effects among PiPr3,
 PiPr2(3,5-(CF3)2C6H3), and PiPr2Me
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6444
_journal_page_last               6450
_journal_paper_doi               10.1021/ic000500t
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C30 H68 Cl4 O2 P4 Ru2'
_chemical_formula_weight         928.715
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method
'minor manual editing of SDT2CIF v. 1.2 BETA  output'
_cell_angle_alpha                90
_cell_angle_beta                 111.7582
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.7729(11)
_cell_length_b                   16.2148(8)
_cell_length_c                   12.5448(6)
_cell_measurement_reflns_used    5980
_cell_measurement_temperature    121(2)
_cell_measurement_theta_max      32.45
_cell_measurement_theta_min      2.64
_cell_volume                     4113.3(4)
_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      121(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  5210
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3
_diffrn_reflns_theta_full        32.5089
_diffrn_reflns_theta_max         32.5089
_diffrn_reflns_theta_min         2.08373
_diffrn_standards_decay_%        0.
_diffrn_standards_interval_time  83
_diffrn_standards_number         316
_exptl_absorpt_coefficient_mu    1.1753
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.892089
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.5
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .30
_refine_diff_density_max         0.56
_refine_diff_density_min         -0.87
_refine_ls_abs_structure_details none
_refine_ls_extinction_coef       -0.000000045(4)
_refine_ls_extinction_expression
;

Larson, A. C. (1967).  Acta Cryst. 23, p. 664.  Eq. (3)

;
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_ref   1.3245
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         5210
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.0021
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w^-1^=\s^2^(F)+(.07F)^2^
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0470
_reflns_number_gt                5210
_reflns_number_total             7418
_reflns_threshold_expression     'Fo^2^> 2.33\s(Fo^2^)'
_cod_data_source_file            ic000500t.cif
_cod_data_source_block           MSC99147
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4320624