Synthesis and Structural Characterization of Metallogermylenes, Cp-Substituted Germylene, and a Germanium(II)-Borane Adduct from Pyridyl-1-azaallyl Germanium(II) Chloride
Leung, Wing-Por; Chiu, Wang-Kin; Mak, Thomas C. W.; Organometallics 31 (2012) 6966–; doi:10.1021/om3007739

data_4079492
_publ_section_title
;
 Synthesis and Structural Characterization of Metallogermylenes,
 Cp-Substituted Germylene, and a Germanium(II)-Borane Adduct from
 Pyridyl-1-azaallyl Germanium(II) Chloride
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              6966
_journal_paper_doi               10.1021/om3007739
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C27 H32 Ge Mo N2 O3 Si2'
_chemical_formula_weight         657.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 94.579(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.921(2)
_cell_length_b                   15.088(2)
_cell_length_c                   26.873(4)
_cell_measurement_temperature    293(2)
_cell_volume                     6030.6(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            20123
_diffrn_reflns_theta_full        28.04
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    1.521
_exptl_absorpt_correction_T_max  0.5813
_exptl_absorpt_correction_T_min  0.4622
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.010(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         9597
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0831
_reflns_number_gt                8336
_reflns_number_total             9597
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3007739_si_001.cif
_cod_data_source_block           p
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        6030.5(15)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               4079492