Borabenzene Adducts of Ylidic Lewis Bases. Syntheses and Structures of 3,5-Me2C5H3BCH2PPh3, 3,5-Me2C5H3BCH(SiMe3)PPh3, and C5H5BN(Ph)PPh31
Zheng, Xiaolai; Wang, Bing; Herberich, Gerhard E.; Organometallics 21 (2002) 1949–; doi:10.1021/om011081q

data_4076764
_publ_section_title
;
 Borabenzene Adducts of Ylidic Lewis Bases. Syntheses and Structures of
 3,5-Me2C5H3BCH2PPh3, 3,5-Me2C5H3BCH(SiMe3)PPh3, and C5H5BN(Ph)PPh31
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1949
_journal_paper_doi               10.1021/om011081q
_journal_volume                  21
_journal_year                    2002
_chemical_compound_source        'see paper'
_chemical_formula_sum            'C32.5 H38 B P Si'
_chemical_formula_weight         498.53
_chemical_name_common            ' compound 5'
_chemical_name_systematic
; (trimethylsilyl)(triphenylphosphonio)methanide-
3,5-dimethylborabenzene
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                84.888(8)
_cell_angle_beta                 82.61(1)
_cell_angle_gamma                81.40(1)
_cell_formula_units_Z            2.00
_cell_length_a                   9.141(2)
_cell_length_b                   10.733(1)
_cell_length_c                   14.701(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    180
_cell_measurement_theta_max      26
_cell_measurement_theta_min      16
_cell_volume                     1410.7(4)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1977)
_computing_data_collection       CAD4_(Enraf-Nonius,_1977)
_computing_data_reduction        PROCESS_MolEN_(Fair,_1990)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Enraf_Nonius_CAD4
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_type           Cu-K\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_av_sigmaI/netI    0.0665
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7731
_diffrn_reflns_theta_full        70.06
_diffrn_reflns_theta_max         69.9
_diffrn_reflns_theta_min         4.2
_diffrn_standards_decay_%        0.42
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.392
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.876
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_density_meas      ?
_exptl_crystal_description       rod
_exptl_crystal_F_000             534
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       not_refined
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    refined_isotropically
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         5321
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1284
_reflns_number_gt                4200
_reflns_number_total             5321
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om011081q.cif
_cod_data_source_block           xz17_061000
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C32.5 H38 B1 P1 Si1'
_cod_database_code               4076764