(3-<i>tert</i>-Butyl isocyanide)-3,8-bis(dimethylphenylphosphine)octahydro-1,2-diarsa-3-pallada-<i>closo</i>-dodecaboron(1+) Hexafluoroantimonate
Ferguson, G.; Li, Y.; Spalding, T. R.; Patterson, J. C.; Acta Crystallographica Section C 51 (1995) 1498–1500; doi:10.1107/S0108270195002198

data_2003741
_publ_section_title
;(3-<i>tert</i>-Butyl
 isocyanide)-3,8-bis(dimethylphenylphosphine)octahydro-1,2-diarsa-3-pallada-<i>closo</i>-dodecaboron(1+)
 Hexafluoroantimonate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1498
_journal_page_last               1500
_journal_paper_doi               10.1107/S0108270195002198
_journal_volume                  51
_journal_year                    1995
_chemical_compound_source        'synthesised by the authors'
_chemical_formula_moiety         '(C21 H39 As2 B9 N P2 Pd) (Sb F6)'
_chemical_formula_structural
'((C4 H9 N C)(P(C H3)2 (C6 H5))2 (Pd As2 B9 H8)) 1+, Sb F6 1-'
_chemical_formula_sum            'C21 H39 As2 B9 F6 N P2 Pd Sb'
_chemical_formula_weight         956.75
_chemical_name_systematic
;
closo-[(3-tert-Butylisocyanide)-3,8-bis(dimethylphenylphosphine)-
octahydro-1,2-diarsenanonaborato(1-)-3-palladium(II)(1+)]
Hexafluoroantimonate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                96.6120(9)
_cell_angle_beta                 102.2910(10)
_cell_angle_gamma                105.039(8)
_cell_formula_units_Z            2
_cell_length_a                   9.9342(8)
_cell_length_b                   13.0495(13)
_cell_length_c                   15.3141(14)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    291(1)
_cell_measurement_theta_max      21.00
_cell_measurement_theta_min      14.50
_cell_volume                     1842.5(3)
_computing_cell_refinement       'Enraf-Nonius SET4 and CELDIM'
_computing_data_collection       'Enraf-Nonius CAD4 (Enraf-Nonius 1992)'
_computing_data_reduction
'DATRD2 in NRCVAX94 (Gabe, Le Page, Charland, Lee & White, 1989)'
_computing_molecular_graphics
;NRCVAX94; PLATON (Spek, 1994a); PLUTON (Spek 1994b); ORTEPII (Johnson,
1976)
;
_computing_publication_material  'NRCVAX94; SHELXL93; WordPerfect'
_computing_structure_refinement  'NRCVAX94; SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       '\q/2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7201
_diffrn_reflns_theta_max         25.90
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        'no decay, variation 1.0'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.136
_exptl_absorpt_correction_T_max  0.7032
_exptl_absorpt_correction_T_min  0.5700
_exptl_absorpt_correction_type   'empirical, 9 \y scans at 4\% steps'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.728
_refine_diff_density_min         '-1.101 e \%A^-3^, 0.95\%A from As2'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.026
_refine_ls_goodness_of_fit_obs   1.216
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         7201
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.027
_refine_ls_restrained_S_obs      1.217
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_obs          0.0430
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0644P)^2^] where P=(Fo^2^+2F~c~^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1176
_refine_ls_wR_factor_obs         0.1071
_reflns_number_observed          4403
_reflns_number_total             7201
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            ab1248.cif
_cod_data_source_block           93-51trs9317
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0644P)^2^] where P=(Fo^2^+2F~c~^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^)+(0.0644P)^2^] where P=(Fo^2^+2F~c~^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2003741