Syntheses, Characterizations, and Coordination Chemistry of the 10-Vertex Phosphadicarbaboranes 6-R-arachno-6,8,9-PC2B7H11 and 6-R-arachno-6,5,7-PC2B7H11
Daewon Hong; Scott E. Rathmill; Patrick J. Carroll; Larry G. Sneddon; Journal of the American Chemical Society 125 (2003) 16058–16073; doi:10.1021/ja037799+

data_4114527
_publ_section_title
;
 Syntheses, Characterizations, and Coordination Chemistry of the 10-Vertex
 Phosphadicarbaboranes 6-R-arachno-6,8,9-PC2B7H11 and
 6-R-arachno-6,5,7-PC2B7H11
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16058
_journal_page_last               16073
_journal_paper_doi               10.1021/ja037799+
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C16 H32 B14 Br2 P2 Pd'
_chemical_formula_weight         703.92
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.100(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.6297(9)
_cell_length_b                   8.5490(10)
_cell_length_c                   19.160(2)
_cell_measurement_temperature    143(1)
_cell_volume                     1412.6(3)
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0152
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8927
_diffrn_reflns_theta_max         28.91
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    3.607
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.896
_refine_diff_density_min         -1.833
_refine_diff_density_rms         0.331
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.231
_refine_ls_goodness_of_fit_obs   1.235
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         8927
_refine_ls_number_restraints     125
_refine_ls_restrained_S_all      1.224
_refine_ls_restrained_S_obs      1.227
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_obs          0.0845
_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^)+(0.1100P)^2^+20.8093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2309
_refine_ls_wR_factor_obs         0.2253
_reflns_number_observed          8441
_reflns_number_total             8927
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja0377992Bsi20030808_011521.cif
_cod_data_source_block           Cmpd_8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+20.8093P] 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^)+(0.1100P)^2^+20.8093P] 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_sg_symbol_H-M      'P 21/n '
_cod_database_code               4114527