Unusual Polybrominated Polypyrazolylborates and Their Copper(I) Complexes: Synthesis, Characterization, and Catalytic Activity
Glen P. A. Yap; Fernando Jove; Juan Urbano; Eleuterio Alvarez; Swiatoslaw Trofimenko; M. Mar Díaz-Requejo; Pedro J. Pérez; Inorganic Chemistry 46 (2007) 780–787; doi:10.1021/ic061714z

data_4307168
_publ_section_title
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Unusual Polybrominated Polypyrazolylborates and Their Copper(I)
Complexes: Synthesis, Characterization, and Catalytic Activity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              780
_journal_page_last               787
_journal_paper_doi               10.1021/ic061714z
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C33 H21 B Br3 Cl4 N6 Tl'
_chemical_formula_weight         1098.27
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.300(5)
_cell_angle_beta                 95.000(5)
_cell_angle_gamma                103.330(5)
_cell_formula_units_Z            2
_cell_length_a                   10.390(4)
_cell_length_b                   11.299(4)
_cell_length_c                   15.977(6)
_cell_measurement_reflns_used    1017
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     1785.9(12)
_computing_cell_refinement       'SHELXTL, Sheldrick (2001)'
_computing_data_collection       'SMART, Bruker (2002)'
_computing_data_reduction        'SHELXTL, Sheldrick (2001)'
_computing_molecular_graphics    'SHELXTL, Sheldrick (2001)'
_computing_publication_material  'SHELXTL, Sheldrick (2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       \w
_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  0.0718
_diffrn_reflns_av_sigmaI/netI    0.0898
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17882
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    8.212
_exptl_absorpt_correction_T_max  0.3722
_exptl_absorpt_correction_T_min  0.2905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick (2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.042
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.945
_refine_diff_density_min         -2.236
_refine_diff_density_rms         0.442
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         8000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0858
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1634P)^2^+9.1447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2260
_refine_ls_wR_factor_ref         0.2284
_reflns_number_gt                7611
_reflns_number_total             8000
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061714zsi20060910_125331.cif
_cod_data_source_block           compound4_(local_labelling_jert041)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
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_cod_original_cell_volume        1785.9(11)
_cod_database_code               4307168