Solid State Structure of {[HC(3,5-Me2pz)3][HB(3,5-Me2pz)3]Cd}{B[3,5-(CF3)2C6H3]4}: Comparison of the Bonding of Tris(pyrazolyl)methane and Tris(pyrazolyl)borate Ligands
Daniel L. Reger; James E. Collins; Arnold L. Rheingold; Louise M. Liable-Sands; Inorganic Chemistry 38 (1999) 3235–3237; doi:10.1021/ic981453w

data_4322115
_publ_contact_author
;
     Dr. D. L. Reger
     Department of Chemistry and Biochemistry
     University of South Carolina
     Columbia, S.C. 29208
     USA
;
_publ_contact_author_email       reger@mail.psc.sc.edu
_publ_contact_author_fax         '+803 777 9521'
_publ_contact_author_phone       '+803 777 2587'
_publ_section_title
;
 Solid State Structure of
 {[HC(3,5-Me2pz)3][HB(3,5-Me2pz)3]Cd}{B[3,5-(CF3)2C6H3]4}: Comparison of
 the Bonding of Tris(pyrazolyl)methane and Tris(pyrazolyl)borate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3235
_journal_page_last               3237
_journal_paper_doi               10.1021/ic981453w
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C63 H56 B2 Cd F24 N12'
_chemical_formula_weight         1571.22
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                108.50(2)
_cell_angle_beta                 96.53(5)
_cell_angle_gamma                103.23(4)
_cell_formula_units_Z            2
_cell_length_a                   10.311(6)
_cell_length_b                   19.045(5)
_cell_length_c                   19.611(6)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    244(2)
_cell_measurement_theta_max      12.36
_cell_measurement_theta_min      3.97
_cell_volume                     3482(3)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      244(2)
_diffrn_measurement_method       'omega/phi 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  0.0719
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_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
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_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        8.83
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_T_max  0.7352
_exptl_absorpt_correction_T_min  0.5746
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
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_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
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_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_obs          0.0601
_refine_ls_shift/esd_max         0.237
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1345
_refine_ls_wR_factor_obs         0.1273
_reflns_number_observed          7409
_reflns_number_total             11987
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981453w.cif
_cod_data_source_block           dlr28
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] 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^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3482.0(25)
_cod_database_code               4322115