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_4088485
_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         'C45 H40 B P'
_chemical_formula_sum            'C45 H40 B P'
_chemical_formula_weight         622.55
_chemical_name_common            'Phenyl 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                66.6893(12)
_cell_angle_beta                 82.5213(12)
_cell_angle_gamma                89.1313(12)
_cell_formula_units_Z            4
_cell_length_a                   10.5235(3)
_cell_length_b                   16.9647(5)
_cell_length_c                   21.1690(7)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.1945
_cell_measurement_theta_min      2.4015
_cell_volume                     3438.50(18)
_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 0.998
_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  0.0401
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            57886
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_min         2.279
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABs
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       prism
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.121
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.069
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         14590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0534P)^2^+1.6012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1261
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11303
_reflns_number_total             14590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00123_si_002.cif
_cod_data_source_block           2
_cod_database_code               4088485
_shelx_estimated_absorpt_t_min   0.963
_shelx_estimated_absorpt_t_max   0.991
_shelxl_version_number           2013-4
_shelx_res_checksum              27591
_shelx_hkl_checksum              78464
_loop
;Comments
Due to presence of the five phenyls on 
the B1 and C1-C4 carbons of the molecule,
it was difficult to assign the position of 
P1 in reference to B1, resulting in disorder. 
Utilizing the PART instruction, we were able to model 
the system with 85% occupancy at P1 and 
15% occupancy at P1A. This disorder thus 
accounts for the majority of the 
Hirshfeld Test errors (PLAT230) as well as 
the PLAT301_ALERT_3_G error detailing the
percentage of disorder in the system. 
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
C161, C167 and C169 (R, R, and S) respectively.
;