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_4084656
_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         'C54 H42 F Ge P3, 2.5(C4 H8 O)'
_chemical_formula_sum            'C64 H62 F Ge O2.5 P3'
_chemical_formula_weight         1055.64
_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'
_cell_angle_alpha                74.147(8)
_cell_angle_beta                 67.510(6)
_cell_angle_gamma                81.619(9)
_cell_formula_units_Z            2
_cell_length_a                   11.9214(13)
_cell_length_b                   13.7238(17)
_cell_length_c                   18.6671(19)
_cell_measurement_reflns_used    9110
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      4.0592
_cell_volume                     2711.5(5)
_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 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
scan:
    Number of images: 720
               Slice: -80.0000 - 100.0000
         Image width: 0.2500
            Exp time: 3.0000
       Rotation axis: Phi
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 35.1618
              2theta: 9.8099
scan:
    Number of images: 200
               Slice: -30.0000 - 20.0000
         Image width: 0.2500
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 0.0000
                 XTD: 35.1618
              2theta: 9.8099
scan:
    Number of images: 200
               Slice: -30.0000 - 20.0000
         Image width: 0.2500
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 90.0000
                 XTD: 35.1618
              2theta: 9.8099
scan:
    Number of images: 200
               Slice: -30.0000 - 20.0000
         Image width: 0.2500
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 180.0000
                 XTD: 35.1618
              2theta: 9.8099

;
_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  0.0511
_diffrn_reflns_av_sigmaI/netI    0.0757
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26988
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.06
_diffrn_source_current           200.0000
_diffrn_source_power             10.0000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_T_max  0.9205
_exptl_absorpt_correction_T_min  0.8170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB(Rigaku, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1104
_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          0.12
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         12173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0684
_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^)+(0.0466P)^2^+3.1093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1487
_reflns_number_gt                9241
_reflns_number_total             12173
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500906f_si_003.cif
_cod_data_source_block           2a
_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/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.
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C64 H62 F Ge O2.50 P3'
_cod_database_code               4084656