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_4076763
_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            'C26 H26 B P'
_chemical_formula_weight         380.28
_chemical_name_common            ' compound 3'
_chemical_name_systematic
' (triphenylphosphonio)methanide-3,5-dimethylborabenzene'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.04(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4.00
_cell_length_a                   9.498(2)
_cell_length_b                   12.950(3)
_cell_length_c                   17.303(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    223
_cell_measurement_theta_max      12
_cell_measurement_theta_min      7
_cell_volume                     2125.3(9)
_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      223
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       Enraf_Nonius_CAD4
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.106
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9050
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         26.0
_diffrn_reflns_theta_min         2.4
_diffrn_standards_decay_%        -10.67
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  0.000
_exptl_absorpt_correction_T_min  0.000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.19
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.95
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.182
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       not_refined
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.704
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         4165
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.704
_refine_ls_R_factor_all          0.1951
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.1053
_reflns_number_gt                1419
_reflns_number_total             4161
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om011081q.cif
_cod_data_source_block           xz19_241100
_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_cell_volume        2125.2(9)
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'C26 H26 B1 P1'
_cod_database_code               4076763