Mono-, di-, and triborylphosphine analogues of triarylphosphines.
Bailey, Jonathan A.; Ploeger, Marten; Pringle, Paul G.; Inorganic chemistry 53 (2014) 7763–7769; doi:10.1021/ic501133n

data_4340311
_publ_section_title
;
 Mono-, di-, and triborylphosphine analogues of triarylphosphines.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7763
_journal_page_last               7769
_journal_paper_doi               10.1021/ic501133n
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C26 H21 B2 N4 P'
_chemical_formula_sum            'C26 H21 B2 N4 P'
_chemical_formula_weight         442.06
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6850(7)
_cell_length_b                   19.4779(11)
_cell_length_c                   8.0751(5)
_cell_measurement_reflns_used    4247
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.91
_cell_measurement_theta_min      2.57
_cell_volume                     2152.5(2)
_computing_cell_refinement       'Apex II (Bruker, 2008)'
_computing_data_collection       'Apex II (Bruker, 2008)'
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_computing_structure_solution    SHELXS
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_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0849
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            35926
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.531
_diffrn_reflns_theta_min         1.045
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       'cut needle'
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 1618 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.01(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4951
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+0.2474P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                4026
_reflns_number_total             4951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501133n_si_002.cif
_cod_data_source_block           jb0182_new
_cod_depositor_comments
'Adding full bibliography for 4340309--4340313.cif.'
_cod_database_code               4340311
_shelxl_version_number           2013-2
_shelx_res_checksum              78322
_shelx_hkl_checksum              63706