Neutral and cationic main group element cages of germanium(ii) with pyrazolyl ligands: solid state structures, DFT calculations and advanced solution NMR investigations
Krummenacher, Ivo; Fernández, Ignacio; Rüegger, Heinz; Weigend, Florian; Breher, Frank; Dalton Transactions  (2009) 5335–5347; doi:10.1039/b901711a

data_7001625
_publ_section_title
;
 Neutral and cationic main group element cages of germanium(ii) with
 pyrazolyl ligands: solid state structures, DFT calculations and
 advanced solution NMR investigations
;
_journal_issue                   27
_journal_name_full               'Dalton Transactions'
_journal_page_first              5335
_journal_page_last               5347
_journal_paper_doi               10.1039/b901711a
_journal_year                    2009
_chemical_formula_moiety         'C20 H4 F24 Ge2 N8'
_chemical_formula_sum            'C20 H4 F24 Ge2 N8'
_chemical_formula_weight         957.49
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.560(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1677(6)
_cell_length_b                   37.262(2)
_cell_length_c                   9.3337(6)
_cell_measurement_reflns_used    28474
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.19
_cell_volume                     2985.4(3)
_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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex with CCD'
_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  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            28474
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    2.195
_exptl_absorpt_correction_T_max  0.4664
_exptl_absorpt_correction_T_min  0.2600
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.130
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular shaped crystal'
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.84
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.41
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         7406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+4.3565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                6291
_reflns_number_total             7406
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b901711a.txt
_cod_data_source_block           Ge2CF3CF3neutral
_cod_original_cell_volume        2985.3(3)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7001625