Investigation of the Reactivity of Hydroxyborate Salts with Group IV Metal Complexes: Synthesis and Structural Characterization of the Zirconium and Hafnium Ionic Complexes [PPN]+[Cp2MMe(OB(C6F5)3)]−
Kelsen, Vinciane; Vallée, Christophe; Jeanneau, Erwann; Bibal, Christine; Santini, Catherine C.; Chauvin, Yves; Olivier-Bourbigou, Hélène; Organometallics 30 (2011) 4284–; doi:10.1021/om2002798

data_4063568
_publ_section_title
;
 Investigation of the Reactivity of Hydroxyborate Salts with Group IV
 Metal Complexes: Synthesis and Structural Characterization of the
 Zirconium and Hafnium Ionic Complexes [PPN]+[Cp2MMe(OB(C6F5)3)]&#x2212;
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4284
_journal_paper_doi               10.1021/om2002798
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         '    C36 H30 N P2, C18 H B F15 O '
_chemical_formula_sum            'C54 H31 B F15 N O P2'
_chemical_formula_weight         1067.57
_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
_cell_angle_alpha                67.3774(9)
_cell_angle_beta                 88.0710(10)
_cell_angle_gamma                64.5140(10)
_cell_formula_units_Z            2
_cell_length_a                   12.7244(3)
_cell_length_b                   14.0170(4)
_cell_length_c                   16.7119(4)
_cell_measurement_reflns_used    11170
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      0.407
_cell_volume                     2452.33(11)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11718
_diffrn_reflns_theta_full        27.942
_diffrn_reflns_theta_max         27.942
_diffrn_reflns_theta_min         1.337
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.28
_refine_ls_extinction_coef       110(20)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0845
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         7391
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.000451
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.392 0.277 0.131 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0890
_refine_ls_wR_factor_gt          0.0526
_refine_ls_wR_factor_ref         0.0502
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              18
_reflns_limit_k_min              -16
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                7993
_reflns_number_total             11718
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0442
_oxford_refine_ls_scale          0.3023(4)
_oxford_reflns_number_all        11679
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            om2002798_si_001.cif
_cod_data_source_block           1VK97
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        '    C54 H31 B F15 N O P2 '
_cod_database_code               4063568