Syntheses and Structural Characterizations of endo-η1-, exo-η1-, η4-, η5-, and η6-Metallaphosphamonocarbaborane Complexes Derived from a Versatile New Polyborane Ligand: exo-6-R-arachno-6,7-PCB8H12
Daniel E. Kadlecek; Alexandra M. Shedlow; Sang Ook Kang; Patrick J. Carroll; Larry G. Sneddon; Journal of the American Chemical Society 125 (2003) 212–220; doi:10.1021/ja020945b

data_4113368
_publ_section_title
;
 Syntheses and Structural Characterizations of endo-\h1-, exo-\h1-, \h4-,
 \h5-, and \h6-Metallaphosphamonocarbaborane Complexes Derived from a
 Versatile New Polyborane Ligand: exo-6-R-arachno-6,7-PCB8H12
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              212
_journal_page_last               220
_journal_paper_doi               10.1021/ja020945b
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C12 H19 B8 Fe P'
_chemical_formula_weight         336.57
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                96.392(3)
_cell_angle_beta                 106.633(2)
_cell_angle_gamma                78.401(2)
_cell_formula_units_Z            2
_cell_length_a                   7.8825(3)
_cell_length_b                   16.0671(6)
_cell_length_c                   6.9036(2)
_cell_measurement_temperature    293(2)
_cell_volume                     819.29(5)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'image plate area detector'
_diffrn_measurement_device_type  'Rigaku R-AXIS IIc'
_diffrn_measurement_method       'phi oscillations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6868
_diffrn_reflns_theta_max         24.95
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    1.002
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.067
_refine_ls_goodness_of_fit_obs   1.081
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2654
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_restrained_S_obs      1.081
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_obs          0.0398
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+0.6591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1074
_refine_ls_wR_factor_obs         0.1046
_reflns_number_observed          2467
_reflns_number_total             2654
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja020945b_3.cif
_cod_data_source_block           cmpd4a(Upenn3067)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+0.6591P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+0.6591P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4113368