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_4113363
_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            'C21 H33 B8 N2 P'
_chemical_formula_weight         430.94
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.5550(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.71360(10)
_cell_length_b                   16.1166(2)
_cell_length_c                   14.49750(10)
_cell_measurement_temperature    200(2)
_cell_volume                     2503.12(4)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_diffrn_ambient_temperature      200(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  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19744
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.145
_refine_ls_goodness_of_fit_obs   1.164
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         4547
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_restrained_S_obs      1.164
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_obs          0.0503
_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^)+(0.0418P)^2^+1.1500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1150
_refine_ls_wR_factor_obs         0.1120
_reflns_number_observed          4203
_reflns_number_total             4547
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja020944j_1.cif
_cod_data_source_block           PSH+3a-(Upenn3149)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+1.1500P] 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^)+(0.0418P)^2^+1.1500P] 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/c '
_cod_database_code               4113363