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_4317796
_publ_contact_author
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  Jose Vicente
Grupo de Quimica Organometalica. Departamento
de Quimica Inorganica, Facultad de Quimica
Universidad de Murcia, apartado 4021
Murcia 30071. Spain
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_publ_contact_author_email       jvs@um.es
_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            'C9 H10 Au B Cl2 N6'
_chemical_formula_weight         480.91
_chemical_name_systematic
;
  ?
;
_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     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 100.219(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.0620(6)
_cell_length_b                   13.1237(9)
_cell_length_c                   11.9099(7)
_cell_measurement_reflns_used    65
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      12.45
_cell_measurement_theta_min      6.07
_cell_volume                     1393.94(16)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_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      298(2)
_diffrn_measurement_device       '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  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4328
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        0.3
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    10.930
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.201
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.292
_exptl_crystal_description       prism
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.108
_refine_diff_density_min         -1.721
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.055
_refine_ls_goodness_of_fit_obs   1.105
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2446
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.022
_refine_ls_restrained_S_obs      1.061
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_obs          0.0378
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0992
_refine_ls_wR_factor_obs         0.0915
_reflns_number_observed          1931
_reflns_number_total             2446
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic011031d_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

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

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

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0558P)^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^)+(0.0558P)^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        1393.9(2)
_cod_database_code               4317796