Bimetallic, Spirocyclic, Methylene-Bridged Carbene Complexes of Rhodium and Palladium Derived by Stepwise Metalations of Lithiated Bis(diphenylphosphoranotrimethylsilylimido)methandiide
Fang, Min; Jones, Nathan D.; Friesen, Kristina; Lin, Guanyang; Ferguson, Michael J.; McDonald, Robert; Lukowski, Robert; Cavell, Ronald G.; Organometallics 28 (2009) 1652–; doi:10.1021/om8005678

data_4068284
_publ_section_title
;
 Bimetallic, Spirocyclic, Methylene-Bridged Carbene Complexes of Rhodium
 and Palladium Derived by Stepwise Metalations of Lithiated
 Bis(diphenylphosphoranotrimethylsilylimido)methandiide
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1652
_journal_paper_doi               10.1021/om8005678
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C43 H60 Li N2 O P2 Rh Si2, 1.5(C6 H6)'
_chemical_formula_sum            'C52 H69 Li N2 O P2 Rh Si2'
_chemical_formula_weight         966.06
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL template'
_cell_angle_alpha                74.0271(11)
_cell_angle_beta                 85.5899(12)
_cell_angle_gamma                67.1842(11)
_cell_formula_units_Z            2
_cell_length_a                   10.9009(9)
_cell_length_b                   13.2220(10)
_cell_length_c                   19.9057(16)
_cell_measurement_reflns_used    5921
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.31
_cell_measurement_theta_min      2.17
_cell_volume                     2541.0(4)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_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  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19717
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.484
_exptl_absorpt_correction_T_max  0.9354
_exptl_absorpt_correction_T_min  0.8685
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Bruker SHELXTL (Bruker, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1018
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         10314
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+0.8504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0968
_reflns_number_gt                8904
_reflns_number_total             10314
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om8005678_si_002.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               4068284