Fusing triphenylphosphine with tetraphenylborate: introducing the 9-phosphatriptycene-10-phenylborate (PTB) anion.
Drover, Marcus W.; Nagata, Koichi; Peters, Jonas C.; Chemical communications (Cambridge, England) 54 (2018) 7916–7919; doi:10.1039/c8cc04321c

data_7125323
_publ_section_title
;
 Fusing triphenylphosphine with tetraphenylborate: introducing the
 9-phosphatriptycene-10-phenylborate (PTB) anion.
;
_journal_issue                   57
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7916
_journal_page_last               7919
_journal_paper_doi               10.1039/c8cc04321c
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C24 H17 B Br3 Co P, 2(C8 H20 N)'
_chemical_formula_sum            'C40 H57 B Br3 Co N2 P'
_chemical_formula_weight         906.31
_chemical_name_systematic        PTBCo(Br)3(NEt4)2
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-02-15
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-16 deposited with the CCDC.
2018-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.679(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5630(10)
_cell_length_b                   16.1347(13)
_cell_length_c                   18.6380(16)
_cell_measurement_reflns_used    9827
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.475
_cell_measurement_theta_min      3.631
_cell_volume                     4058.6(6)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Apex Duo II'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            55074
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.934
_diffrn_reflns_theta_min         2.382
_exptl_absorpt_coefficient_mu    7.362
_exptl_absorpt_correction_T_max  0.357
_exptl_absorpt_correction_T_min  0.266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1263 before and 0.0953 after correction.
The Ratio of minimum to maximum transmission is 0.7059.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       plate
_exptl_crystal_F_000             1852
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         4.819
_refine_diff_density_min         -1.387
_refine_diff_density_rms         0.346
_refine_ls_extinction_coef       0.0022(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   2.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         8674
_refine_ls_number_restraints     393
_refine_ls_restrained_S_all      2.025
_refine_ls_R_factor_all          0.1737
_refine_ls_R_factor_gt           0.1602
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4098
_refine_ls_wR_factor_ref         0.4362
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7710
_reflns_number_total             8674
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04321c2.cif
_cod_data_source_block           mkt_a
_cod_database_code               7125323
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.425
_shelx_estimated_absorpt_t_min   0.307
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.706(4)
 0.294(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C35(H35A,H35B), C37(H37A,H37B), C39(H39A,H39B), C25(H25A,
 H25B), C27(H27A,H27B), C29(H29A,H29B), C31(H31A,H31B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C22(H22), C23(H23), C24(H24),
  C21(H21)
5.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C40(H40A,H40B,
 H40C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C32(H32A,
 H32B,H32C)
;
_olex2_submission_special_instructions 'No special instructions were received'