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_4307171
_publ_section_title
;
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_moiety         '2(C34 H31 B Br3 Cu N8), C2 H3 N'
_chemical_formula_sum            'C70 H65 B2 Br6 Cu2 N17'
_chemical_formula_weight         1772.55
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 106.492(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.878(2)
_cell_length_b                   10.3822(11)
_cell_length_c                   19.223(2)
_cell_measurement_reflns_used    6972
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.51
_cell_measurement_theta_min      2.25
_cell_volume                     3612.6(7)
_computing_cell_refinement       'SAINT+ v. 6.04 (Bruker-AXS, 2001)'
_computing_data_collection       'SMART v. 5.625 (Bruker-AXS, 2001)'
_computing_data_reduction        'SAINT+ v. 6.04 (Bruker-AXS, 2001)'
_computing_molecular_graphics    'xp program, SHELXTL v. 6.10, BRUKER, 2000'
_computing_publication_material  'XCIF program, SHELXTL v.6.10, Bruker, 2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker Smart APEX CCD system'
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_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  0.0827
_diffrn_reflns_av_sigmaI/netI    0.0681
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            53795
_diffrn_reflns_theta_full        26.48
_diffrn_reflns_theta_max         26.48
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.961
_exptl_absorpt_correction_T_max  0.3718
_exptl_absorpt_correction_T_min  0.1828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS v. 2.03: Area-Detector Absorption Correction.
 (1997-2001) Bruker-AXS within SAINT+ package, v. 6.04
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.299
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         7122
_refine_ls_number_restraints     353
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0697
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+98.8301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1475
_reflns_number_gt                5467
_reflns_number_total             7122
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061714zsi20060910_125445.cif
_cod_data_source_block           compound10_(local_labelling_ea08506b)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_database_code               4307171