Reactivity of Divalent Germanium Alkoxide Complexes Is in Sharp Contrast to the Heavier Tin and Lead Analogues
Lorenzo Ferro; Peter B. Hitchcock; Martyn P. Coles; J. Robin Fulton; Inorganic Chemistry 51 (2012) 1544–1551; doi:10.1021/ic201841m

data_4328159
_publ_section_title
;
 Reactivity of Divalent Germanium Alkoxide Complexes Is in Sharp Contrast
 to the Heavier Tin and Lead Analogues
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1544
_journal_page_last               1551
_journal_paper_doi               10.1021/ic201841m
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C33 H50 Ge N2 O'
_chemical_formula_sum            'C33 H50 Ge N2 O'
_chemical_formula_weight         563.34
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2011-10-12T21:30:00-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 121.696(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3507(3)
_cell_length_b                   16.6088(3)
_cell_length_c                   16.9602(3)
_cell_measurement_reflns_used    33030
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     3199.82(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.156159E-1
_diffrn_orient_matrix_UB_12      -0.585803E-1
_diffrn_orient_matrix_UB_13      -0.36816E-2
_diffrn_orient_matrix_UB_21      0.495395E-1
_diffrn_orient_matrix_UB_22      0.13172E-1
_diffrn_orient_matrix_UB_23      -0.363517E-1
_diffrn_orient_matrix_UB_31      0.586803E-1
_diffrn_orient_matrix_UB_32      0.44691E-2
_diffrn_orient_matrix_UB_33      0.58882E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44895
_diffrn_reflns_theta_full        25.86
_diffrn_reflns_theta_max         25.86
_diffrn_reflns_theta_min         3.42
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.983
_exptl_absorpt_correction_T_max  0.8046
_exptl_absorpt_correction_T_min  0.7359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       prism
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         6043
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+1.9595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                5144
_reflns_number_total             6043
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201841m_si_001_3.cif
_cod_data_source_block           (2c)-nov507
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4328159