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_4307170
_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         'C32 H25 B Br6 Cu N7, C H2 Cl2'
_chemical_formula_sum            'C33 H27 B Br6 Cl2 Cu N7'
_chemical_formula_weight         1146.33
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.948(9)
_cell_length_b                   10.025(4)
_cell_length_c                   34.381(15)
_cell_measurement_reflns_used    6797
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.55
_cell_measurement_theta_min      2.81
_cell_volume                     7220(5)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0729
_diffrn_reflns_av_sigmaI/netI    0.1095
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            86556
_diffrn_reflns_theta_full        27.22
_diffrn_reflns_theta_max         27.22
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    7.432
_exptl_absorpt_correction_T_max  0.4081
_exptl_absorpt_correction_T_min  0.2797
_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    2.109
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4416
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.704
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         15544
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1117
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+5.6062P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1400
_reflns_number_gt                9326
_reflns_number_total             15544
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061714zsi20060910_125427.cif
_cod_data_source_block           compound7_(local_labelling_ea08406x)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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               4307170