Syntheses, Crystallographic/Computational Characterizations, and Reactions of the First 10-Vertex arachno- and nido-Phosphamonocarbaboranes
Alexandra M. Shedlow; Daniel E. Kadlecek; Jude C. Clapper; Scott E. Rathmill; Patrick J. Carroll; Larry G. Sneddon; Journal of the American Chemical Society 125 (2003) 200–211; doi:10.1021/ja020944j

data_4113364
_publ_section_title
;
 Syntheses, Crystallographic/Computational Characterizations, and
 Reactions of the First 10-Vertex arachno- and
 nido-Phosphamonocarbaboranes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              200
_journal_page_last               211
_journal_paper_doi               10.1021/ja020944j
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C16 H31 B8 N2 P'
_chemical_formula_weight         368.88
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 101.898(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9467(2)
_cell_length_b                   15.8609(2)
_cell_length_c                   10.3485(1)
_cell_measurement_temperature    210(2)
_cell_volume                     2239.98(5)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_diffrn_ambient_temperature      210(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     0.71069
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16686
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.094
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.272
_refine_ls_goodness_of_fit_obs   1.293
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.272
_refine_ls_restrained_S_obs      1.293
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_obs          0.0710
_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^)+(0.0389P)^2^+1.5371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1433
_refine_ls_wR_factor_obs         0.1391
_reflns_number_observed          3634
_reflns_number_total             3968
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja020944j_2.cif
_cod_data_source_block           PSH+3b-(Upenn3158)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+1.5371P] 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^)+(0.0389P)^2^+1.5371P] 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 21/n '
_cod_database_code               4113364