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_4113365
_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            'C25 H43 B8 N2 O P S'
_chemical_formula_weight         537.12
_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                 104.249(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.445(2)
_cell_length_b                   10.723(2)
_cell_length_c                   25.458(5)
_cell_measurement_temperature    143(1)
_cell_volume                     3028.2(10)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_diffrn_ambient_temperature      143(2)
_diffrn_measurement_device       'CCD area detector'
_diffrn_measurement_device_type  'Rigaku Mercury'
_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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            19957
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.720
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.119
_refine_ls_goodness_of_fit_obs   1.176
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         6720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_restrained_S_obs      1.176
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_obs          0.0728
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+4.0587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1449
_refine_ls_wR_factor_obs         0.1339
_reflns_number_observed          5293
_reflns_number_total             6720
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja020944j_3.cif
_cod_data_source_block           PSH+5a-(Upenn3201)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+4.0587P] 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^)+(0.0352P)^2^+4.0587P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-scans' was replaced
with the value 'multi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        3028.2(9)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               4113365