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_4309036
_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         'C22 H30 Ge N2 O4'
_chemical_formula_sum            'C22 H30 Ge N2 O4'
_chemical_formula_weight         459.07
_chemical_name_systematic
; 
Bis[N-methyl-(2-oxy-2-phenylethyl)-(2-oxyethyl)amine]germanium
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6124(1)
_cell_length_b                   11.6124(1)
_cell_length_c                   15.5183(2)
_cell_measurement_reflns_used    8939
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.870
_cell_measurement_theta_min      2.480
_cell_volume                     2092.61(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1K'
_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  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15351
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    1.495
_exptl_absorpt_correction_T_max  0.8649
_exptl_absorpt_correction_T_min  0.7542
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0246
_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^)+(0.0339P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0559
_refine_ls_wR_factor_ref         0.0570
_reflns_number_gt                2362
_reflns_number_total             2540
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic048165msi20041228_094930_1.cif
_cod_data_source_block           k
_cod_database_code               4309036