2,4,6-Triphenylphosphinine and 2,4,6-triphenylposphabarrelene revisited: synthesis, reactivity and coordination chemistry.
Rigo, M.; Sklorz, J. A. W.; Hatje, N.; Noack, F.; Weber, M.; Wiecko, J.; Müller, C; Dalton transactions (Cambridge, England : 2003) 45 (2016) 2218–2226; doi:10.1039/c5dt03609g

data_7037221
_publ_section_title
;
 2,4,6-Triphenylphosphinine and 2,4,6-triphenylposphabarrelene revisited:
 synthesis, reactivity and coordination chemistry.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2218
_journal_page_last               2226
_journal_paper_doi               10.1039/c5dt03609g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C50 H34 O4 P2 W, 2(C2 H3 N)'
_chemical_formula_sum            'C54 H40 N2 O4 P2 W'
_chemical_formula_weight         1026.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-09-09
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2015-09-15 deposited with the CCDC.
2015-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.7420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.1358(14)
_cell_length_b                   11.5350(6)
_cell_length_c                   15.4712(7)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.312
_cell_measurement_theta_min      2.697
_cell_volume                     4514.6(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32070
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.360
_diffrn_reflns_theta_min         2.635
_exptl_absorpt_coefficient_mu    2.679
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6306
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1068 before and 0.0675 after correction.
The Ratio of minimum to maximum transmission is 0.8456.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       plate
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.971
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.011(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         9939
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0360P)^2^+1.1400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0679
_reflns_Friedel_coverage         0.999
_reflns_friedel_fraction_full    0.998
_reflns_friedel_fraction_max     0.994
_reflns_number_gt                9315
_reflns_number_total             9939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03609g2.cif
_cod_data_source_block           FN02B
_cod_depositor_comments
'Adding full bibliography for 7037218--7037221.cif.'
_cod_database_code               7037221
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22),
  C23(H23), C25(H25), C27(H27), C30(H30), C31(H31), C32(H32), C33(H33),
 C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43),
  C44(H44), C45(H45), C46(H46)
2.b Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              20645
_olex2_submission_special_instructions 'No special instructions were received'