Novel pyrazolate coordination modes and unusual Tl · · · Tl or Tl-π-(phenyl) interactions in the crystal structures of [{Tl3(Ph2pz)3}n], [{Tl4(Ph2pz)4}n], [{Tl4(Ph2pz)3(OH)}2] and [{Tl4(MePhpz)3(OH)}n] (Ph2pz = 3,5-diphenylpyrazolate; MePhpz = 3-methyl-5-phenylpyrazolate)
Deacon, Glen B.; Delbridge, Ewan E.; Forsyth, Craig M.; Skelton, Brian W.; White, Allan H.; Journal of the Chemical Society, Dalton Transactions  (2000) 745–; doi:10.1039/a909048g

data_7009167
_publ_section_title
;
 Novel pyrazolate coordination modes and unusual
 Tl&#x200A;&#x200A;&#x00B7;&#x2005;&#x00B7;&#x2005;&#x00B7;&#x200A;&#x200A;Tl
 or Tl-\p-(phenyl) interactions in the crystal structures of
 [{Tl3(Ph2pz)3}n], [{Tl4(Ph2pz)4}n], [{Tl4(Ph2pz)3(OH)}2] and
 [{Tl4(MePhpz)3(OH)}n] (Ph2pz&#x2005;=&#x2005;3,5-diphenylpyrazolate;
 MePhpz&#x2005;=&#x2005;3-methyl-5-phenylpyrazolate)
;
_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              745
_journal_paper_doi               10.1039/a909048g
_journal_year                    2000
_chemical_formula_sum            'C64 H54 N8 O2 Tl4'
_chemical_formula_weight         1784.63
_chemical_name_systematic
; 
 [(3,5-diphenylpyrazolato)thallium(I)].1,2-dimethoxyethane 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.37(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.367(2)
_cell_length_b                   17.566(4)
_cell_length_c                   28.465(6)
_cell_measurement_temperature    123(2)
_cell_volume                     5674(2)
_computing_cell_refinement       'DENZO-SMN (Otwinowski and Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius B.V., 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski and Minor, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (Siemans, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device_type  'Enraf Nonius CCD'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0611
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            12968
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.93
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    11.378
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.089
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3336
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         4.825
_refine_diff_density_min         -2.911
_refine_diff_density_rms         0.304
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         12968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+74.3534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1439
_reflns_number_gt                9643
_reflns_number_total             12968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a909048g.txt
_cod_data_source_block           ewantl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+74.3534P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+74.3534P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      p_1_21/n_1
_cod_database_code               7009167