Reactivity of Phosphaboradibenzofulvene toward Hydrogen, Acetonitrile, Benzophenone, and 2,3-Dimethylbutadiene
Breunig, Jens Michael; Hübner, Alexander; Bolte, Michael; Wagner, Matthias; Lerner, Hans-Wolfram; Organometallics 32 (2013) 6792–; doi:10.1021/om400553j

data_4081803
_publ_section_title
;
 Reactivity of Phosphaboradibenzofulvene toward Hydrogen, Acetonitrile,
 Benzophenone, and 2,3-Dimethylbutadiene
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6792
_journal_paper_doi               10.1021/om400553j
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C44 H58 B2 N2 P2, C7 H8'
_chemical_formula_sum            'C51 H66 B2 N2 P2'
_chemical_formula_weight         790.61
_chemical_name_systematic        ?
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                98.241(17)
_cell_angle_beta                 94.212(17)
_cell_angle_gamma                97.434(16)
_cell_formula_units_Z            2
_cell_length_a                   11.697(2)
_cell_length_b                   12.687(3)
_cell_length_c                   15.914(3)
_cell_measurement_reflns_used    9278
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.1
_cell_measurement_theta_min      3.3
_cell_volume                     2307.4(8)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1539
_diffrn_reflns_av_unetI/netI     0.2116
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22847
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.762
_diffrn_reflns_theta_min         3.275
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_description       rod
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         8659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.856
_refine_ls_R_factor_all          0.1921
_refine_ls_R_factor_gt           0.0717
_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^)+(0.0391P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1639
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3393
_reflns_number_total             8659
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400553j_si_002.cif
_cod_data_source_block           wa1687
_cod_database_code               4081803
_shelx_estimated_absorpt_t_min   0.977
_shelx_estimated_absorpt_t_max   0.995
_shelxl_version_number           2013-3
_shelx_res_checksum              42133
_shelx_hkl_checksum              39413