Noveltert-Butyl-tris(3-hydrocarbylpyrazol-1-yl)borate Ligands: Synthesis, Spectroscopic Studies, and Coordination Chemistry#
Graziani, Olivier; Hamon, Paul; Thépot, Jean-Yves; Toupet, Loïc; Szilágyi, Petra Á.; Molnár, Gábor; Bousseksou, Azzedine; Tilset, Mats; Hamon, Jean-René; Inorganic Chemistry 45 (2006) 5661–5674; doi:10.1021/ic060458n

data_4332502
_publ_section_title
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 Noveltert-Butyl-tris(3-hydrocarbylpyrazol-1-yl)borate Ligands:&#x00A0;
 Synthesis, Spectroscopic Studies, and Coordination Chemistry#
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_journal_issue                   14
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5661
_journal_page_last               5674
_journal_paper_doi               10.1021/ic060458n
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C16 H24 B F3 Fe0.5 N6 P0.5'
_chemical_formula_weight         411.63
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                   10.0554(1)
_cell_length_b                   18.6230(3)
_cell_length_c                   20.5137(3)
_cell_measurement_temperature    293(2)
_cell_volume                     3841.43(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Nonius (1999)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'PLATON_(Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97_(Altomare & al., 1998)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 19.24
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  Nonius_KappaCCD
_diffrn_measurement_method       'Area detector scans (see text)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4402
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0033(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0549
_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^)+(0.1125P)^2^+2.6260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1629
_refine_ls_wR_factor_ref         0.1828
_reflns_number_gt                3263
_reflns_number_total             4402
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060458nsup3.cif
_cod_data_source_block           phtp21
_cod_depositor_comments
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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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      Pbcn
_cod_original_formula_sum        'C16 H24 B F3 Fe0.50 N6 P0.50'
_cod_database_code               4332502