Reaction of a 2,4,6-triphenylphosphinine ferrate anion with electrophiles: a new route to phosphacyclohexadienyl complexes.
Hoidn, Christian M.; Wolf, Robert; Dalton transactions (Cambridge, England : 2003) 45 (2016) 8875–8884; doi:10.1039/c6dt00336b

data_7039080
_publ_section_title
;
 Reaction of a 2,4,6-triphenylphosphinine ferrate anion with
 electrophiles: a new route to phosphacyclohexadienyl complexes.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8875
_journal_page_last               8884
_journal_paper_doi               10.1039/c6dt00336b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C34 H35 Fe P'
_chemical_formula_sum            'C34 H35 Fe P'
_chemical_formula_weight         530.44
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-01-20 deposited with the CCDC.
2016-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.3153(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.89052(5)
_cell_length_b                   16.24733(7)
_cell_length_c                   17.19538(11)
_cell_measurement_reflns_used    43418
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.3860
_cell_measurement_theta_min      3.7040
_cell_volume                     2726.76(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega -112.00  -14.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  -57.0000   30.0000 98

  2 omega   17.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8939  -57.0000 -180.0000 52

  3 omega   45.00   95.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8939 -125.0000   60.0000 50

  4 omega   34.00  118.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -125.0000  -60.0000 84

  5 omega   83.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   30.0000   60.0000 75

  6 omega   32.00  121.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -125.0000  120.0000 89

  7 omega   23.00  102.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000  -30.0000 79

  8 omega   74.00  154.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000  150.0000 80

  9 omega -120.00   -7.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  -77.0000  -90.0000 113

 10 omega -117.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  -37.0000  120.0000 102

 11 omega   73.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000  -60.0000 85

 12 omega   73.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000   90.0000 85

 13 omega   32.00   77.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000  150.0000 45

 14 omega   79.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000 -120.0000 79

 15 omega  -70.00   33.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939   57.0000 -180.0000 103

 16 omega  -70.00   33.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939   57.0000   30.0000 103

 17 omega   32.00   77.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000   60.0000 45

 18 omega   79.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000    0.0000 79

 19 omega   77.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000  -90.0000 81

 20 omega   29.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  -30.0000 40

 21 omega -120.00   -7.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  -77.0000  120.0000 113

 22 omega -120.00   -7.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  -77.0000    0.0000 113

 23 omega   23.00  109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000  150.0000 86

 24 omega   73.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000   60.0000 85

 25 omega   79.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000 -150.0000 79

 26 omega   32.00   77.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000  -60.0000 45

 27 omega -120.00   -7.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  -77.0000 -150.0000 113

 28 omega    2.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8939 -125.0000  -60.0000 96

 29 omega   73.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000  120.0000 85

 30 omega   73.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000    0.0000 85

 31 omega   28.00  141.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -77.0000  -60.0000 113

 32 omega   32.00   77.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000    0.0000 45

 33 omega -117.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  -37.0000 -150.0000 102

 34 omega  -11.00   89.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8939 -110.0000  128.0000 100

 35 omega   73.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000   30.0000 85

 36 omega   32.00   77.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000  120.0000 45

 37 omega   73.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000  -90.0000 85

 38 omega   77.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000 -120.0000 81

 39 omega -115.00  -11.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  -57.0000  120.0000 104

 40 omega -120.00   -7.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  -77.0000   30.0000 113

 41 omega   32.00   77.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000 -180.0000 45

 42 omega   73.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000 -120.0000 85

 43 omega   73.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000 -180.0000 85

 44 omega   77.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000    0.0000 81

 45 omega -117.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  -37.0000  -90.0000 102

 46 omega -115.00  -11.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  -57.0000 -150.0000 104

 47 omega   77.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000  150.0000 81

 48 omega   77.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000   60.0000 81

 49 omega   77.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000  120.0000 81

 50 omega   29.00  115.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -110.0000  128.0000 86

 51 omega -117.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  -37.0000  150.0000 102

 52 omega   -5.00  122.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8939   19.0000    0.0000 127

 53 omega   77.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000  -60.0000 81

 54 omega   77.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000   90.0000 81

 55 omega   77.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000 -180.0000 81

 56 omega   77.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000  -30.0000 81

 57 omega -120.00   -7.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  -77.0000  -30.0000 113

 58 omega -117.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  -37.0000 -180.0000 102

 59 omega   28.00  141.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -77.0000 -180.0000 113

 60 omega   73.00  111.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000  -30.0000 38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0063183000
_diffrn_orient_matrix_UB_12      -0.0923431000
_diffrn_orient_matrix_UB_13      -0.0193114000
_diffrn_orient_matrix_UB_21      0.1556850000
_diffrn_orient_matrix_UB_22      0.0070556000
_diffrn_orient_matrix_UB_23      0.0013373000
_diffrn_orient_matrix_UB_31      0.0252049000
_diffrn_orient_matrix_UB_32      -0.0202505000
_diffrn_orient_matrix_UB_33      0.0887250000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            78382
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.567
_diffrn_reflns_theta_min         3.767
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.128
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.3957
_exptl_crystal_size_mid          0.2794
_exptl_crystal_size_min          0.1335
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         5489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+1.3533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0776
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5289
_reflns_number_total             5489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00336b2.cif
_cod_data_source_block           cmh037_mp
_cod_depositor_comments
'Adding full bibliography for 7039074--7039080.cif.'
_cod_database_code               7039080
_chemical_oxdiff_formula         C34H35FeP
_chemical_oxdiff_usercomment     Hexan-Fraktion
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.023) H4(0.023) H6A(0.044) H6B(0.044) H6C(0.044) H12A(0.07)
 H12B(0.07) H12C(0.07) H13A(0.099) H13B(0.099) H13C(0.099) H14A(0.091)
 H14B(0.091) H14C(0.091) H15A(0.064) H15B(0.064) H15C(0.064) H16A(0.045)
 H16B(0.045) H16C(0.045) H18(0.028) H19(0.035) H20(0.041) H21(0.048) H22(0.037)
 H24(0.032) H25(0.038) H26(0.041) H27(0.041) H28(0.033) H30(0.029) H31(0.036)
 H32(0.039) H33(0.037) H34(0.03)
 Fixed X: H2(0.0217) H4(0.3577) H6A(0.0927) H6B(0.2244) H6C(0.1269)
 H12A(0.5039) H12B(0.5907) H12C(0.6192) H13A(0.1638) H13B(0.2852) H13C(0.2996)
 H14A(0.1003) H14B(0.1376) H14C(0.0558) H15A(0.3803) H15B(0.3694) H15C(0.237)
 H16A(0.6443) H16B(0.6507) H16C(0.5693) H18(0.2122) H19(0.1076) H20(-0.0955)
 H21(-0.1953) H22(-0.0899) H24(-0.0136) H25(-0.1162) H26(-0.0694) H27(0.0837)
 H28(0.1907) H30(0.5331) H31(0.7635) H32(0.8856) H33(0.7742) H34(0.5447)
 Fixed Y: H2(0.7174) H4(0.8549) H6A(0.8813) H6B(0.933) H6C(0.906) H12A(0.6089)
 H12B(0.5526) H12C(0.6475) H13A(0.522) H13B(0.4624) H13C(0.5254) H14A(0.6009)
 H14B(0.5128) H14C(0.5738) H15A(0.7442) H15B(0.6556) H15C(0.7013) H16A(0.7276)
 H16B(0.6801) H16C(0.763) H18(0.654) H19(0.55) H20(0.4929) H21(0.5435)
 H22(0.6458) H24(0.7286) H25(0.7731) H26(0.9034) H27(0.9876) H28(0.9422)
 H30(0.916) H31(0.9436) H32(0.8864) H33(0.802) H34(0.7722)
 Fixed Z: H2(0.4453) H4(0.5291) H6A(0.2559) H6B(0.2863) H6C(0.345)
 H12A(0.3635) H12B(0.4268) H12C(0.4262) H13A(0.3942) H13B(0.4255) H13C(0.3583)
 H14A(0.5948) H14B(0.5678) H14C(0.5069) H15A(0.6651) H15B(0.6996) H15C(0.659)
 H16A(0.5343) H16B(0.6142) H16C(0.6007) H18(0.2338) H19(0.155) H20(0.1793)
 H21(0.2828) H22(0.3634) H24(0.5653) H25(0.6691) H26(0.7218) H27(0.6717)
 H28(0.5696) H30(0.5106) H31(0.5175) H32(0.4267) H33(0.3284) H34(0.3221)
;
_shelx_res_checksum              96124
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'