Contribution of the nido-[7,8-C~2~B~9~H~10~]^-^ Anion to the Chemical Stability, Basicity, and ^31^P NMR Chemical Shift in nido-o-Carboranylmonophosphines
Francesc Teixidor; Rosario Núñez; Clara Viñas; Reijo Sillanpää; Raikko Kivekäs; Inorganic Chemistry 40 (2001) 2587–2594; doi:10.1021/ic000858p

data_4319649
_publ_contact_author
;   
     Dr. Clara Vi\~nas
     Institut de Ci\`encia de Materials de Barcelona     
     C.S.C.I.
     Campus U.A.B.
     08193 Bellaterra
     Spain
;
_publ_contact_author_email       clara@icmab.es
_publ_contact_author_fax         '+ 34 3 5805729'
_publ_contact_author_phone       '+ 34 3 5801853'
_publ_section_title
;
 Contribution of the nido-[7,8-C~2~B~9~H~10~]^-^ Anion to the Chemical
 Stability, Basicity, and ^31^P NMR Chemical Shift in
 nido-o-Carboranylmonophosphines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2587
_journal_page_last               2594
_journal_paper_doi               10.1021/ic000858p
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'N C16 H36, C20 H25 B9 O P'
_chemical_formula_sum            'C36 H61 B9 N O P'
_chemical_formula_weight         652.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.884(7)
_cell_length_b                   21.485(4)
_cell_length_c                   13.404(7)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      13.26
_cell_measurement_theta_min      7.75
_cell_volume                     3998(3)
_computing_cell_refinement
;
MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 
1995)
;
_computing_data_collection
;
MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 
1995)
;
_computing_data_reduction
;
Texsan Process (Molecular Structure Corporation, 1989)
;
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku AFC5S'
_diffrn_measurement_method       w\--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2148
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3929
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.3(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         3929
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.2505
_refine_ls_R_factor_gt           0.0752
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1987
_reflns_number_gt                1526
_reflns_number_total             3929
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000858p_2.cif
_cod_data_source_block           '[NBu~4~][7-P(O)Ph~2~-8-Ph-7,8-C~2~B~9~H~10~]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+0.0000P] 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^)+(0.0725P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4319649