Bis[tris(3,5-dimethyl-1<i>H</i>-pyrazol-1-yl-κ<i>N</i>^2^)methyl]sodium trifluoromethanesulfonate
Lyubartseva, Ganna; Parkin, Sean; Mallik, Uma Prasad; Acta Crystallographica Section E 68 (2012) m973–; doi:10.1107/S1600536812028413

data_2235653
_publ_section_title
;
 Bis[tris(3,5-dimethyl-1<i>H</i>-pyrazol-1-yl-\k<i>N</i>^2^)methyl]sodium
 trifluoromethanesulfonate
;
_journal_coeditor_code           TK5119
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m973
_journal_paper_doi               10.1107/S1600536812028413
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Na (C16 H22 N6)2] C F3 O3 S'
_chemical_formula_moiety         'C32 H44 N12 Na +, C F3 O3 S -'
_chemical_formula_sum            'C33 H44 F3 N12 Na O3 S'
_chemical_formula_weight         768.85
_chemical_name_systematic
;
Bis[tris(3,5-dimethyl-1<i>H</i>-pyrazol-1-yl-\k<i>N</i>^2^)methyl]sodium
trifluoromethanesulfonate
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.5917(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.05790(10)
_cell_length_b                   12.57330(10)
_cell_length_c                   16.4386(2)
_cell_measurement_reflns_used    4496
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1872.05(3)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and local procedures'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 9.1
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w scans at fixed \c = 55\%'
_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  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47745
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.62
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.165
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[SCALEPACK (Otwinowski & Minor, 1997) and XABS2 (Parkin <i>et al.</i>
1995)]
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.268
_refine_ls_abs_structure_details nd
_refine_ls_abs_structure_Flack   0.50(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         8385
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0596P)^2^+0.4716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1121
_reflns_number_gt                7036
_reflns_number_total             8385
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk5119.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               2235653
_cod_database_fobs_code          2235653