The monoclinic polymorph of <i>rac</i>-5,7,7,12,12,14-hexamethyl-1,4,8,11-tetraazoniacyclotetradecane bis(hexafluorogermanate) tetrahydrate
Fonari, Marina S.; Simonov, Yurii A.; Chumakov, Yurii M.; Bocelli, Gabriele; Ganin, Eduard V.; Gelmboldt, Vladimir O.; Acta Crystallographica Section C 59 (2003) m168–m170; doi:10.1107/S0108270103005869

data_2013252
_publ_section_title
;
 The monoclinic polymorph of
 <i>rac</i>-5,7,7,12,12,14-hexamethyl-1,4,8,11-tetraazoniacyclotetradecane
 bis(hexafluorogermanate) tetrahydrate
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m168
_journal_page_last               m170
_journal_paper_doi               10.1107/S0108270103005869
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '(C16 H40 N4) [Ge F6]2, 4H2 O'
_chemical_formula_moiety         'C16 H40 N4 4+, 2F6 Ge 2-, 4H2 O'
_chemical_formula_sum            'C16 H48 F12 Ge2 N4 O4'
_chemical_formula_weight         733.76
_chemical_melting_point          70
_chemical_name_common
;
(H4-tet b) bis(hexafluorogermanate)tetrahydrate
;
_chemical_name_systematic
;
rac-5,7,7,12,12,14-hexamethyl-
1,4,8,11-tetraazoniacyclotetradecane bis(hexafluorogermanate)
tetrahydrate
;
_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                 96.28(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.5650(19)
_cell_length_b                   16.522(3)
_cell_length_c                   9.0210(18)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.16
_cell_measurement_theta_min      5.63
_cell_volume                     1417.1(5)
_computing_cell_refinement       'BELLETTI (Belletti, 1996)'
_computing_data_collection       'LEHMAN (Lehman & Larsen, 1974)'
_computing_data_reduction        LEHMAN
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
;
Phillips PW1100 four-circle diffractometer
;
_diffrn_measurement_method       \w-2\q
_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  0.0148
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4350
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         3.19
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.230
_exptl_absorpt_correction_T_max  0.6640
_exptl_absorpt_correction_T_min  0.6056
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'North et al. (1968)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.621
_refine_ls_extinction_coef       0.0035(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4137
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0437P)^2^+0.0000P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0717
_reflns_number_gt                3251
_reflns_number_total             4137
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn1019.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2013252
_cod_database_fobs_code          2013252