Multiple Silicon-Hydrogen Bond Activations at Adjacent Rhodium and Iridium Centers
Md Hosnay Mobarok; Okemona Oke; Michael J. Ferguson; Robert McDonald; Martin Cowie; Inorganic Chemistry 49 (2010) 11556–11572; doi:10.1021/ic1017196

data_4317341
_publ_section_title
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 Multiple Silicon-Hydrogen Bond Activations at Adjacent Rhodium and
 Iridium Centers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11556
_journal_page_last               11572
_journal_paper_doi               10.1021/ic1017196
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C72 H72 Ir O4 P4 Rh Si2'
_chemical_formula_weight         1476.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.7210(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.9511(12)
_cell_length_b                   15.0138(10)
_cell_length_c                   24.0458(16)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.43
_cell_measurement_theta_min      2.28
_cell_volume                     6436.1(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0683
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            52248
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         26.78
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    2.508
_exptl_absorpt_correction_T_max  0.9196
_exptl_absorpt_correction_T_min  0.5487
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2984
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
Attempts to refine peaks of residual electron density as 
disordered or partial-occupancy solvent tetrahydrofuran carbon or oxygen 
atoms were unsuccessful.  The data were corrected for disordered electron 
density through use of the SQUEEZE procedure (Sluis, P. van der; Spek, A. 
L. Acta Crystallogr. 1990, A46, 194-201) as implemented in PLATON (Spek, 
A. L. Acta Crystallogr. 1990, A46, C34; Spek, A. L. J. Appl. Cryst. 2003, 
36, 7-13.  PLATON - a multipurpose crystallographic tool.  Utrecht 
University, Utrecht, The Netherlands).  A total solvent-accessible void 
volume of 1150 cubic angstroms  with a total electron count of 350 
(consistent with approximately 8 molecules of solvent tetrahydrofuran, 
or 2 molecules per formula unit of the RhIr complex) was found in the unit 
cell.
;
_refine_diff_density_max         1.041
_refine_diff_density_min         -1.185
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         13711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0415P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0838
_reflns_number_gt                10053
_reflns_number_total             13711
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic1017196_si_002_4.cif
_cod_data_source_block           compound8b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4317341