Synthesis, X-ray Diffraction Studies, and DFT Calculations on Hexacoordinated Germanium Derivatives: The Case of Germaspirobis(ocanes)
Sergey S. Karlov; Elmira Kh. Lermontova; Maxim V. Zabalov; Anastasia A. Selina; Andrei V. Churakov; Judith A. K. Howard; Mikhail Yu. Antipin; Galina S. Zaitseva; Inorganic Chemistry 44 (2005) 4879–4886; doi:10.1021/ic048165m

data_4309037
_publ_contact_author
; Dr Galina S. Zaitseva
  Department of Chemistry, Moscow State University
  Leninskie Gory, Moscow 119899, Russia
;
_publ_contact_author_email       zait@org.chem.msu.su
_publ_section_title
;
Synthesis, X-ray Diffraction Studies, and DFT Calculations on
Hexacoordinated Germanium Derivatives: The Case of Germaspirobis(ocanes)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4879
_journal_page_last               4886
_journal_paper_doi               10.1021/ic048165m
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C20 H26 Ge N2 O4, C7 H8'
_chemical_formula_sum            'C27 H34 Ge N2 O4'
_chemical_formula_weight         523.15
_chemical_name_systematic
; 
Bis(N-phenyl-diethanolamine)germanium toluene solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 118.135(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.0253(7)
_cell_length_b                   18.4791(7)
_cell_length_c                   17.4343(7)
_cell_measurement_reflns_used    7473
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.021
_cell_measurement_theta_min      2.204
_cell_volume                     4836.9(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       \w
_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  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27669
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    1.303
_exptl_absorpt_correction_T_max  0.7805
_exptl_absorpt_correction_T_min  0.7805
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.568
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         11658
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1109
_reflns_number_gt                7700
_reflns_number_total             11658
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic048165msi20041228_094930_2.cif
_cod_data_source_block           z
_cod_database_code               4309037