Anion directed supramolecular architecture of pyrazole based ionic salts
Singh, Udai P.; Kashyap, Sujata; Singh, Hari Ji; Butcher, Ray J.; CrystEngComm 13 (2011) 4110–; doi:10.1039/c0ce00820f

data_7205807
_publ_section_title
;
 Anion directed supramolecular architecture of pyrazole based ionic
 salts
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              4110
_journal_paper_doi               10.1039/c0ce00820f
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety
;
8(C15 H13 N2), 4(H O4 S), 2(O4 S), 3(H2 O)
;
_chemical_formula_sum            'C120 H114 N16 O27 S6'
_chemical_formula_weight         2404.63
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 104.689(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.7258(7)
_cell_length_b                   20.1708(8)
_cell_length_c                   20.1033(7)
_cell_measurement_reflns_used    7634
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      1.05
_cell_volume                     5776.1(4)
_computing_cell_refinement       'Bruker kappa Apex'
_computing_data_collection       'Bruker kappa Apex'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker XSHELL (Sheldrick, 2008)'
_computing_publication_material  'Bruker XSHELL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Apex 2 CCD area detector'
_diffrn_measurement_method       '\w 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  0.0864
_diffrn_reflns_av_sigmaI/netI    0.1161
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            107003
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    0.202
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2516
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.28(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1545
_refine_ls_number_reflns         27489
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0588
_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^)+(0.0484P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1235
_reflns_number_gt                17694
_reflns_number_total             27489
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c0ce00820f.txt
_cod_data_source_block           ups898
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7205807