Synthesis, Geometry, and Bonding Nature of Heptacoordinate Compounds of Silicon and Germanium Featuring Three Phosphine Donors
Kameo, Hajime; Kawamoto, Tatsuya; Sakaki, Shigeyoshi; Bourissou, Didier; Nakazawa, Hiroshi; Organometallics 33 (2014) 6557–; doi:10.1021/om500906f

data_4084660
_publ_section_title
;
 Synthesis, Geometry, and Bonding Nature of Heptacoordinate Compounds of
 Silicon and Germanium Featuring Three Phosphine Donors
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6557
_journal_paper_doi               10.1021/om500906f
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C55 H45 Ge P3, C H2 Cl2'
_chemical_formula_sum            'C56 H47 Cl2 Ge P3'
_chemical_formula_weight         956.34
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
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_cell_angle_beta                 92.827(2)
_cell_angle_gamma                110.444(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1068(19)
_cell_length_b                   14.253(3)
_cell_length_c                   16.483(3)
_cell_measurement_reflns_used    6066
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.4797
_cell_measurement_theta_min      2.0193
_cell_volume                     2386.0(8)
_computing_cell_refinement       'CrystalClear (Rigaku, 2001)'
_computing_data_collection       'CrystalClear (Rigaku, 2001)'
_computing_data_reduction        '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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
scan:
    Number of images: 600
               Slice: -80.0000 - 100.000
         Image width: 0.3000
            Exp time: 12.0000
       Rotation axis: Phi
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 45.4313
              2theta: 20.0953
scan:
    Number of images: 160
               Slice: -20.0000 - 28.0000
         Image width: 0.3000
            Exp time: 12.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 0.0000
                 XTD: 45.4313
              2theta: 20.0953
scan:
    Number of images: 160
               Slice: -20.0000 - 28.0000
         Image width: 0.3000
            Exp time: 12.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 90.0000
                 XTD: 45.4313
              2theta: 20.0953
scan:
    Number of images: 160
               Slice: -20.0000 - 28.0000
         Image width: 0.3000
            Exp time: 12.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 180.0000
                 XTD: 45.4313
              2theta: 20.0953
scan:
    Number of images: 160
               Slice: -20.0000 - 28.0000
         Image width: 0.3000
            Exp time: 12.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 270.0000
                 XTD: 45.4313
              2theta: 20.0953
scan:
    Number of images: 157
               Slice: -20.0000 - 27.1000
         Image width: 0.3000
            Exp time: 12.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 45.4313
              2theta: 20.0953
scan:
    Number of images: 157
               Slice: -20.0000 - 27.1000
         Image width: 0.3000
            Exp time: 12.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 45.4313
              2theta: 20.0953
scan:
    Number of images: 157
               Slice: -20.0000 - 27.1000
         Image width: 0.3000
            Exp time: 12.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 45.4313
              2theta: 20.0953
scan:
    Number of images: 157
               Slice: -20.0000 - 27.1000
         Image width: 0.3000
            Exp time: 12.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 270.0000
                 XTD: 45.4313
              2theta: 20.0953

;
_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 and \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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29418
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.43
_diffrn_source_current           250.0000
_diffrn_source_power             13.7500
_diffrn_source_voltage           55.0000
_exptl_absorpt_coefficient_mu    0.892
_exptl_absorpt_correction_T_max  0.9321
_exptl_absorpt_correction_T_min  0.8418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB(Rigaku, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             988
_exptl_crystal_preparation
'mounted on the CryoLoop with Palaton oil and placed in N2 stream at 200(2) K'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.806
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         10897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0583P)^2^+1.5310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1375
_reflns_number_gt                8607
_reflns_number_total             10897
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500906f_si_003.cif
_cod_data_source_block           7b
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 4084655--4084660.cif.
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_cod_original_cell_volume        2386.0(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4084660