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_4081720
_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 H49 B2 Ge P3'
_chemical_formula_sum            'C51 H49 B2 Ge P3'
_chemical_formula_weight         850.03
_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                 111.850(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   46.246(6)
_cell_length_b                   9.4173(14)
_cell_length_c                   21.274(3)
_cell_measurement_reflns_used    4377
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.91
_cell_measurement_theta_min      2.21
_cell_volume                     8600(2)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1211
_diffrn_reflns_av_sigmaI/netI    0.1124
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            55524
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.860
_exptl_absorpt_correction_T_max  0.9502
_exptl_absorpt_correction_T_min  0.8634
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3544
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         9850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1133
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0263P)^2^+7.3800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1156
_reflns_number_gt                5944
_reflns_number_total             9850
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400186m_si_002.cif
_cod_data_source_block           2GeBH3
_cod_original_cell_volume        8599(2)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4081720