Bis(amido)cyclodiphosph(III)azane Hafnium Complexes and Their Activation by Tris(perfluorophenyl)borane
Axenov, Kirill V.; Klinga, Martti; Leskelä, Markku; Repo, Timo; Organometallics 24 (2005) 1336–; doi:10.1021/om0492303

data_4075726
_publ_section_title
;
 Bis(amido)cyclodiphosph(III)azane Hafnium Complexes and Their Activation
 by Tris(perfluorophenyl)borane
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1336
_journal_paper_doi               10.1021/om0492303
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C36 H42 B F15 Hf N4 P2'
_chemical_formula_sum            'C36 H42 B F15 Hf N4 P2'
_chemical_formula_weight         1066.98
_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           SHELX97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.561(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.168(1)
_cell_length_b                   19.986(1)
_cell_length_c                   17.984(1)
_cell_measurement_reflns_used    29711
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      3.21
_cell_volume                     4251.6(5)
_computing_cell_refinement       'COLLECT (Nonius, 2002)'
_computing_data_collection       'COLLECT (Nonius, 2002)'
_computing_data_reduction        'COLLECT (Nonius, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELX97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi & omega scans'
_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  0.0653
_diffrn_reflns_av_sigmaI/netI    0.0889
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29711
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.21
_exptl_absorpt_coefficient_mu    2.627
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            light_yellow
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.512
_refine_diff_density_min         -2.515
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         9645
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0580P)^2^+0.1500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1211
_reflns_number_gt                6258
_reflns_number_total             9645
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0492303si20041005_102149.cif
_cod_data_source_block           308
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4075726