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_7001628
_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 H12 F9 Ge2 N6, C F3 O3 S'
_chemical_formula_sum            'C16 H12 F12 Ge2 N6 O3 S'
_chemical_formula_weight         741.56
_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                 96.056(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.7923(5)
_cell_length_b                   14.6965(8)
_cell_length_c                   40.138(2)
_cell_measurement_reflns_used    32897
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.75
_cell_measurement_theta_min      2.04
_cell_volume                     5157.5(5)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            32897
_diffrn_reflns_theta_full        24.75
_diffrn_reflns_theta_max         24.75
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    2.531
_exptl_absorpt_correction_T_max  0.4712
_exptl_absorpt_correction_T_min  0.4712
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular shaped crystal'
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     799
_refine_ls_number_reflns         8798
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+16.5127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1028
_reflns_number_gt                7906
_reflns_number_total             8798
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b901711a.txt
_cod_data_source_block           Ge2MeCF3cat
_cod_original_cell_volume        5157.6(5)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7001628