Reactivity of a Phosphaalkyne with Pentaarylboroles
Barnard, Jonathan H.; Yruegas, Sam; Couchman, Shannon A.; Wilson, David J. D.; Dutton, Jason L.; Martin, Caleb D.; Organometallics 35 (2016) 929–; doi:10.1021/acs.organomet.6b00123

data_4088484
_publ_section_title
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 Reactivity of a Phosphaalkyne with Pentaarylboroles
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_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              929
_journal_paper_doi               10.1021/acs.organomet.6b00123
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C51 H44 B P, 0.5(C6 H14)'
_chemical_formula_sum            'C54 H51 B P'
_chemical_formula_weight         741.72
_chemical_name_common            'Biphenyl BP cluster'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                95.795(2)
_cell_angle_beta                 107.259(2)
_cell_angle_gamma                107.969(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3812(8)
_cell_length_b                   12.7207(9)
_cell_length_c                   15.9938(12)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.81
_cell_measurement_theta_min      2.343
_cell_volume                     2055.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            57530
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.343
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_description       prism
_exptl_crystal_F_000             790
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         9075
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+0.6677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1092
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7173
_reflns_number_total             9075
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00123_si_002.cif
_cod_data_source_block           2Ph
_cod_database_code               4088484
_shelx_estimated_absorpt_t_min   0.960
_shelx_estimated_absorpt_t_max   0.988
_shelxl_version_number           2013-4
_shelx_res_checksum              87319
_shelx_hkl_checksum              99347
_loop
;Comments
The level G alerts PLAT343_ALERT_2_G for C4 and C5
(larger angles) seem to result from the 
coordination to P1 and subsequent distortion of 
tetrahedral symmetry. The PLAT779_ALERT_4_G similarly
results from a short bond angle between C4-P1-B1
and is relevant to the structure. Additionally,
the structure contains two chiral centers at
C3 and C5 (R and S) respectively. The n-hexane solvate
was modeled accordingly without disorder.
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