Synthesis and Reactivity of Rhodium Complexes Bearing [E(o-C6H4PPh2)3]-Type Tetradentate Ligands (E = Si, Ge, and Sn)
Kameo, Hajime; Ishii, Sho; Nakazawa, Hiroshi; Organometallics 31 (2012) 2212–; doi:10.1021/om2011276

data_4076370
_publ_section_title
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 Synthesis and Reactivity of Rhodium Complexes Bearing
 [E(o-C6H4PPh2)3]-Type Tetradentate Ligands (E = Si, Ge, and Sn)
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              2212
_journal_paper_doi               10.1021/om2011276
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C54 H42 Cl P3 Sn'
_chemical_formula_sum            'C54 H42 Cl P3 Sn'
_chemical_formula_weight         937.93
_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                 90.936(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8010(6)
_cell_length_b                   24.4370(12)
_cell_length_c                   14.0419(7)
_cell_measurement_reflns_used    11332
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      4.0511
_cell_volume                     4392.0(4)
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
scan:
    Number of images: 600
               Slice: -80.0000 - 100.000
         Image width: 0.3000
            Exp time: 5.0000
       Rotation axis: Phi
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 55.2103
              2theta: 24.7922
scan:
    Number of images: 200
               Slice: -15.0000 - 45.0000
         Image width: 0.3000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 0.0000
                 XTD: 55.2103
              2theta: 24.7922
scan:
    Number of images: 200
               Slice: -15.0000 - 45.0000
         Image width: 0.3000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 90.0000
                 XTD: 55.2103
              2theta: 24.7922
scan:
    Number of images: 200
               Slice: -15.0000 - 45.0000
         Image width: 0.3000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 180.0000
                 XTD: 55.2103
              2theta: 24.7922
scan:
    Number of images: 200
               Slice: -15.0000 - 45.0000
         Image width: 0.3000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 270.0000
                 XTD: 55.2103
              2theta: 24.7922

;
_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  0.0703
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33682
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.05
_diffrn_source_current           250.0000
_diffrn_source_power             12.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_T_max  0.8908
_exptl_absorpt_correction_T_min  0.7977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1912
_exptl_crystal_preparation
'mounted on the CryoLoop with Palaton oil and placed in N2 stream at 200(2) K'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         9881
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+5.3365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1251
_reflns_number_gt                9298
_reflns_number_total             9881
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2011276_si_002.cif
_cod_data_source_block           SnCl
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4076370