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_4088486
_publ_section_title
;
 Reactivity of a Phosphaalkyne with Pentaarylboroles
;
_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         'C40 H29 B'
_chemical_formula_sum            'C40 H29 B'
_chemical_formula_weight         520.44
_chemical_name_common            B-Biphenylborole
_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                68.210(2)
_cell_angle_beta                 88.182(2)
_cell_angle_gamma                85.905(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0877(6)
_cell_length_b                   11.9227(7)
_cell_length_c                   12.2107(7)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.8925
_cell_measurement_theta_min      2.5655
_cell_volume                     1495.01(15)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0318
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            46902
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.521
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_description       prism
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.540
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;Comments
In reference to the level G alerts
PLAT605_ALERT_4_G and PLAT869_ALERT_4_G, 
the unit cell contains 1 
methylene chloride molecule 
on an inversion center 
which has been treated
as a diffuse contribution to the overall 
scattering without specific atom
positions by SQUEEZE/PLATON. 
The level C alert PLAT369_ALERT_2_C
results from PLATON evaluating the 
structure as aromatic when the molecule 
is actually antiaromatic. The C2-C3 bond
(1.53 \%A) is a single bond in this case.
;
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6594
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0452P)^2^+0.4533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1047
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5578
_reflns_number_total             6594
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00123_si_002.cif
_cod_data_source_block           1Ph
_cod_database_code               4088486
_shelx_estimated_absorpt_t_min   0.966
_shelx_estimated_absorpt_t_max   0.987
_shelxl_version_number           2013-4
_shelx_res_checksum              78816
_shelx_hkl_checksum              30655
_platon_squeeze_void_probe_radius 1.20