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_7125327
_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
'C52 H52 B2 Br Co N2 P2, C8 H20 N, 4(C2 H3 N), C2 H9 N'
_chemical_formula_sum            'C70 H93 B2 Br Co N8 P2'
_chemical_formula_weight         1268.92
_chemical_name_systematic        PTBCo(Br)(NCMe)2(NEt4)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.9634(18)
_cell_length_b                   17.7060(13)
_cell_length_c                   29.773(2)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      55.955
_cell_measurement_theta_min      2.969
_cell_volume                     13686.9(17)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Apex Duo II'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.3423
_diffrn_reflns_av_unetI/netI     0.1213
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            49683
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        56.482
_diffrn_reflns_theta_max         56.482
_diffrn_reflns_theta_min         2.968
_exptl_absorpt_coefficient_mu    3.436
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.4289
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1144 before and 0.0823 after correction.
The Ratio of minimum to maximum transmission is 0.5694.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       block
_exptl_crystal_F_000             5368
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.435
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.00002(2)
_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   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         4624
_refine_ls_number_restraints     375
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.2300
_refine_ls_R_factor_gt           0.1730
_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^)+(0.1714P)^2^+557.0297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4104
_refine_ls_wR_factor_ref         0.4570
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2652
_reflns_number_total             4624
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04321c2.cif
_cod_data_source_block           nix4
_cod_original_cell_volume        13686.8(17)
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               7125327
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.683
_shelx_estimated_absorpt_t_min   0.532
_olex2_refinement_description
;
1. 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
2. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(N6)
\\sim Ueq, Uanis(C33) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
3. 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
4. Others
 Fixed Sof: H26A(1.5) H26B(1.5) H26C(1.5) H28A(1.5) H28B(1.5) H28C(1.5)
 H34A(1.5) H34B(1.5) H34C(1.5)
5.a Secondary CH2 refined with riding coordinates:
 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),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23),
  C24(H24)
5.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C32(H32A,H32B,
 H32C), C38(H38A,H38B,H38C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C)
;
_olex2_submission_special_instructions 'No special instructions were received'