Supramolecular anion binding by the [ZnCl(HpztBu)3]+ cation (HpztBu = 5-tert-butylpyrazole)
Renard, Sylvie L.; Kilner, Colin A.; Fisher, Julie; Halcrow, Malcolm A.; Journal of the Chemical Society, Dalton Transactions  (2002) 4206–; doi:10.1039/b207541p

data_7012110
_publ_section_title
;
 Supramolecular anion binding by the [ZnCl(HpztBu)3]+ cation (HpztBu =
 5-tert-butylpyrazole)
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4206
_journal_paper_doi               10.1039/b207541p
_journal_year                    2002
_chemical_formula_moiety         'C21 H36 Cl N6 Zn, B F4, C H2 Cl2'
_chemical_formula_sum            'C22 H38 B Cl3 F4 N6 Zn'
_chemical_formula_weight         645.11
_chemical_name_systematic
; 
Chloro-tris[5-tertbutylpyrazole]zinc(II) tetrafluoroborate 
dichloromethane solvate
;
_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                 116.4774(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5359(3)
_cell_length_b                   10.7282(2)
_cell_length_c                   18.5742(3)
_cell_measurement_reflns_used    30436
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.45
_cell_volume                     3127.82(10)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       'Area detector 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  0.0674
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30436
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    1.087
_exptl_absorpt_correction_T_max  0.7022
_exptl_absorpt_correction_T_min  0.4767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Using multiple and symmetry-related data measurements via the program SORTAV
See R.H. Blessing, Acta Cryst (1995), A51, 33-38 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Rectangular prism'
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       0.0140(16)
_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   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         7131
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+2.0036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1496
_reflns_number_gt                5769
_reflns_number_total             7131
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207541p.txt
_cod_data_source_block           sr10
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3127.83(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7012110