Synthesis of Tris- and Tetrakis(pyrazol-1-yl)borate Gold(III) Complexes. Crystal Structures of [Au{κ2-N,N'-BH(Pz)3}Cl2] (pz = Pyrazol-1-yl) and [Au{κ2-N,N'-B(Pz)4}(κ2-C,N-C6H4CH2NMe2-2)]ClO4.CHCl3
José Vicente; María Teresa Chicote; Rita Guerrero; Ulrich Herber; Delia Bautista; Inorganic Chemistry 41 (2002) 1870–1875; doi:10.1021/ic011031d

data_4317797
_publ_section_title
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 Synthesis of Tris- and Tetrakis(pyrazol-1-yl)borate Gold(III) Complexes.
 Crystal Structures of [Au{\k2-N,N'-BH(Pz)3}Cl2] (pz = Pyrazol-1-yl) and
 [Au{\k2-N,N'-B(Pz)4}(\k2-C,N-C6H4CH2NMe2-2)]ClO4.CHCl3
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1870
_journal_page_last               1875
_journal_paper_doi               10.1021/ic011031d
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C22 H25 Au B Cl4 N9 O4'
_chemical_formula_weight         829.09
_chemical_name_systematic
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  ?
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_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5602(9)
_cell_length_b                   16.1203(18)
_cell_length_c                   21.7920(19)
_cell_measurement_reflns_used    65
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      12.36
_cell_measurement_theta_min      4.22
_cell_volume                     3007.1(5)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Siemens P4'
_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  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0603
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            5599
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        1.6
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.293
_exptl_absorpt_correction_T_max  0.97091
_exptl_absorpt_correction_T_min  0.43108
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.590
_refine_diff_density_min         -1.480
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.117(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         5269
_refine_ls_number_restraints     443
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.108
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+1.2553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1140
_reflns_number_gt                3959
_reflns_number_total             5269
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011031d_2.cif
_cod_data_source_block           3CHCl3
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'Psi-scans' was replaced
with 'psi-scan' value.

'_symmetry_cell_setting' value 'Orthorhombic'
changed to 'orthorhombic' according to the built-in table from CIF
Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_database_code               4317797