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_7001626
_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         '2(C20 H16 F12 Ge2 N8), 3(C7 H8)'
_chemical_formula_sum            'C61 H56 F24 Ge4 N16'
_chemical_formula_weight         1759.58
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.454(2)
_cell_angle_beta                 89.557(2)
_cell_angle_gamma                83.108(2)
_cell_formula_units_Z            1
_cell_length_a                   9.0216(8)
_cell_length_b                   10.9980(10)
_cell_length_c                   18.9911(17)
_cell_measurement_reflns_used    15787
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.24
_cell_volume                     1792.5(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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0648
_diffrn_reflns_av_sigmaI/netI    0.1002
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15787
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    1.774
_exptl_absorpt_correction_T_max  0.7407
_exptl_absorpt_correction_T_min  0.5520
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular shaped crystal'
_exptl_crystal_F_000             878
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         7031
_refine_ls_number_restraints     239
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0530P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                4471
_reflns_number_total             7031
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b901711a.txt
_cod_data_source_block           Ge2MeCF3neutral
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7001626