Synthesis of Zwitterionic Group 14 Centered Complexes: Traditional Coordination and Unusual Insertion Chemistry
Weicker, Sarah A.; Dube, Jonathan W.; Ragogna, Paul J.; Organometallics 32 (2013) 6681–; doi:10.1021/om400186m

data_4081718
_publ_section_title
;
 Synthesis of Zwitterionic Group 14 Centered Complexes: Traditional
 Coordination and Unusual Insertion Chemistry
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6681
_journal_paper_doi               10.1021/om400186m
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C51 H46 B Ge P3'
_chemical_formula_sum            'C51 H46 B Ge P3'
_chemical_formula_weight         835.19
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 94.478(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   42.541(8)
_cell_length_b                   9.3569(18)
_cell_length_c                   21.260(4)
_cell_measurement_reflns_used    2611
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.75
_cell_measurement_theta_min      2.23
_cell_volume                     8437(3)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.1317
_diffrn_reflns_av_sigmaI/netI    0.1453
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            36345
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         0.96
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.875
_exptl_absorpt_correction_T_max  0.9575
_exptl_absorpt_correction_T_min  0.8850
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3472
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.689
_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7725
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1554
_refine_ls_R_factor_gt           0.0750
_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^)+(0.0821P)^2^+19.1648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1715
_refine_ls_wR_factor_ref         0.2065
_reflns_number_gt                4187
_reflns_number_total             7725
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400186m_si_002.cif
_cod_data_source_block           2Ge
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4081718