Si-C bond cleavage by hydride complexes of rhodium and iridium: comparison of Si-C(sp(2)) and Si-C(sp(3)) activation.
Kameo, Hajime; Ishii, Sho; Nakazawa, Hiroshi; Dalton transactions (Cambridge, England : 2003) 42 (2013) 4663–4669; doi:10.1039/c3dt32896a

data_7022727
_publ_section_title
;
 Si-C bond cleavage by hydride complexes of rhodium and iridium:
 comparison of Si-C(sp(2)) and Si-C(sp(3)) activation.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4663
_journal_page_last               4669
_journal_paper_doi               10.1039/c3dt32896a
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C57 H48 Ir O1.0 P3 Si, 0.5(C4 H10 O)'
_chemical_formula_sum            'C59 H53 Ir O1.5 P3 Si'
_chemical_formula_weight         1099.21
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 91.887(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.104(3)
_cell_length_b                   21.128(5)
_cell_length_c                   19.248(5)
_cell_measurement_reflns_used    14168
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      4.0350
_cell_volume                     4920(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2001)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 7.32
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
scan:
Number of images: 600
Slice: -80.0000 - 100.0000
Image width: 0.3000
Exp time: 15.0000
Rotation axis: Phi
Omega: 0.0000
Chi: 0.0000
Phi: 0.0000
XTD: 45.2693
2theta: 19.8001
scan:
Number of images: 160
Slice: -20.0000 - 28.0000
Image width: 0.3000
Exp time: 15.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 90.0000
Phi: 0.0000
XTD: 45.2693
2theta: 19.8001
scan:
Number of images: 160
Slice: -20.0000 - 28.0000
Image width: 0.3000
Exp time: 15.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 90.0000
Phi: 90.0000
XTD: 45.2693
2theta: 19.8001
scan:
Number of images: 160
Slice: -20.0000 - 28.0000
Image width: 0.3000
Exp time: 15.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 90.0000
Phi: 180.0000
XTD: 45.2693
2theta: 19.8001
scan:
Number of images: 160
Slice: -20.0000 - 28.0000
Image width: 0.3000
Exp time: 15.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 90.0000
Phi: 270.0000
XTD: 45.2693
2theta: 19.8001
;
_diffrn_measurement_device       'Mercury CCD (2x2 bin mode)'
_diffrn_measurement_device_details 'AFC7: Eulerian 3-circle'
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       '\w or \f'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38992
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.04
_diffrn_source_current           280.0000
_diffrn_source_power             16.8000
_diffrn_source_voltage           60.0000
_exptl_absorpt_coefficient_mu    2.878
_exptl_absorpt_correction_T_max  0.9186
_exptl_absorpt_correction_T_min  0.5331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             2220
_exptl_crystal_preparation
'mounted on the CryoLoop with Palaton oil and placed in N2 stream at 200(2) K'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.446
_refine_diff_density_min         -1.203
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.230
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         11200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.230
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+11.3965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0927
_reflns_number_gt                10356
_reflns_number_total             11200
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt32896a.txt
_cod_data_source_block           6c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7022727