[(tBu2PCH2SiMe2)2N]RuMe2: Synthesis and Reactivity of an Unsaturated Ruthenium Dialkyl Radical Species
Ingleson, Michael J.; Pink, Maren; Huffman, John C.; Fan, Hongjun; Caulton, Kenneth G.; Organometallics 25 (2006) 1112–1119; doi:10.1021/om0508536

data_4074751
_publ_section_title
;
 [(tBu2PCH2SiMe2)2N]RuMe2: Synthesis and Reactivity of an
 Unsaturated Ruthenium Dialkyl Radical Species
;
_journal_coden_ASTM              ORGND7
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1112
_journal_page_last               1119
_journal_paper_doi               10.1021/om0508536
_journal_volume                  25
_journal_year                    2006
_chemical_formula_structural     'RuCl2(C20H51NP2Si2); 1/3C5H12'
_chemical_formula_sum            'C23.66667 H56 I2 N P2 Ru Si2'
_chemical_formula_weight         827.68
_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_date             09/09/2005
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.910(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   12.533(3)
_cell_length_b                   17.061(4)
_cell_length_c                   47.050(11)
_cell_measurement_reflns_used    1984
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.36
_cell_volume                     10048(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    'Reciprocal Net (http://recipnet.org)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
'   0.30 degree frames measured for 15.16 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  0.0670
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            178943
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    2.492
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  .912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker-AXS SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular fragment'
_exptl_crystal_F_000             4956
_exptl_crystal_id                MSC05237
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.522
_refine_diff_density_min         -1.423
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     992
_refine_ls_number_reflns         23214
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+16.9037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                17820
_reflns_number_total             23214
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0508536si20051223_104905.cif
_cod_data_source_block           05237
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

2026-02-27
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C71 H168 I6 N3 P6 Ru3 Si6'
_cod_original_formula_weight         2483.05
_cod_original_formula_units_Z            4
_cod_original_cell_volume        10047(4)
_cod_original_sg_symbol_H-M      'P2(1)/c  '
_cod_database_code               4074751