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_7001627
_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         'C15 H3 F18 Ge2 N6, C F3 O3 S'
_chemical_formula_sum            'C16 H3 F21 Ge2 N6 O3 S'
_chemical_formula_weight         903.48
_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                 127.789(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.664(1)
_cell_length_b                   11.6115(6)
_cell_length_c                   15.4412(8)
_cell_measurement_reflns_used    11541
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      2.19
_cell_volume                     2786.2(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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11541
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    2.408
_exptl_absorpt_correction_T_max  0.4948
_exptl_absorpt_correction_T_min  0.3079
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular shaped crystal'
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         5899
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0262
_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^)+(0.0535P)^2^+0.2682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0685
_reflns_number_gt                5758
_reflns_number_total             5899
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b901711a.txt
_cod_data_source_block           Ge2CF3CF3cat
_cod_original_cell_volume        2786.3(3)
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               7001627