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_7039075
_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         'C33 H33 Fe P'
_chemical_formula_sum            'C33 H33 Fe P'
_chemical_formula_weight         516.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 103.8168(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.68583(10)
_cell_length_b                   12.90255(8)
_cell_length_c                   19.40989(15)
_cell_measurement_reflns_used    21618
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.4160
_cell_measurement_theta_min      4.1060
_cell_volume                     2598.69(4)
_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 0.989
_diffrn_measurement_details
;
  1 omega  -98.00  -62.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  125.0000   60.0000 36

  2 omega -104.00  -16.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  -37.0000    0.0000 88

  3 omega  -66.00   -8.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939   37.0000 -180.0000 58

  4 omega   72.00  114.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8939  148.0000  -63.0000 42

  5 omega   43.00   86.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000  -60.0000 43

  6 omega   77.00  148.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000  -30.0000 71

  7 omega   36.00   62.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000 -120.0000 26

  8 omega   35.00   67.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  150.0000 32

  9 omega   35.00  114.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -125.0000 -120.0000 79

 10 omega  124.00  158.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000   30.0000 34

 11 omega   39.00   68.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000 -150.0000 29

 12 omega   57.00  119.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -125.0000   30.0000 62

 13 omega   37.00   63.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  -60.0000 26

 14 omega   43.00   69.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000 -150.0000 26

 15 omega   28.00  102.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000 -120.0000 74

 16 omega -115.00  -11.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  -57.0000  -90.0000 104

 17 omega -115.00  -59.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939 -148.0000 -111.0000 56

 18 omega -115.00  -11.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  -57.0000 -180.0000 104

 19 omega -120.00   -7.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  -77.0000  120.0000 113

 20 omega   79.00  158.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000 -180.0000 79

 21 omega   77.00  158.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000  120.0000 81

 22 omega   32.00   77.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000   60.0000 45

 23 omega   29.00   69.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  -30.0000 40

 24 omega   73.00  158.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000 -150.0000 85

 25 omega   28.00  141.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -77.0000   60.0000 113

 26 omega   76.00  158.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   30.0000   60.0000 82

 27 omega   76.00  158.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   30.0000  -60.0000 82

 28 omega -120.00   -7.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  -77.0000    0.0000 113

 29 omega -120.00   -7.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  -77.0000 -120.0000 113

 30 omega  -98.00   -2.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  125.0000 -150.0000 96

 31 omega  -98.00   -2.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8939  125.0000   30.0000 96

 32 omega   73.00  158.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000   90.0000 85

 33 omega   29.00   69.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000   90.0000 40

 34 omega   23.00  109.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000    0.0000 86

 35 omega   77.00  158.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000  -60.0000 81

 36 omega   73.00  158.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000   60.0000 85

 37 omega   73.00  158.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000 -180.0000 85
;
_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      -0.0044894000
_diffrn_orient_matrix_UB_12      0.0047450000
_diffrn_orient_matrix_UB_13      0.0787050000
_diffrn_orient_matrix_UB_21      0.0126300000
_diffrn_orient_matrix_UB_22      -0.1188168000
_diffrn_orient_matrix_UB_23      0.0049824000
_diffrn_orient_matrix_UB_31      0.1478729000
_diffrn_orient_matrix_UB_32      0.0102767000
_diffrn_orient_matrix_UB_33      0.0215217000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38029
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.682
_diffrn_reflns_theta_min         4.152
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.367
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.779
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.2421
_exptl_crystal_size_mid          0.1187
_exptl_crystal_size_min          0.0892
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         5187
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0390P)^2^+1.4097P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0785
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4867
_reflns_number_total             5187
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00336b2.cif
_cod_data_source_block           cmh034_mp
_cod_depositor_comments
'Adding full bibliography for 7039074--7039080.cif.'
_cod_database_code               7039075
_chemical_oxdiff_formula         C33H33FeP
_chemical_oxdiff_usercomment     Hexan-Fraktion
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.023) H4(0.022) H25(0.034) H26(0.032) H23(0.027) H27(0.028)
 H29(0.028) H21(0.031) H1(0.027) H17(0.036) H12A(0.047) H12B(0.047) H12C(0.047)
 H24(0.033) H20(0.038) H15A(0.047) H15B(0.047) H15C(0.047) H30(0.034)
 H11A(0.048) H11B(0.048) H11C(0.048) H33(0.034) H31(0.042) H13A(0.043)
 H13B(0.043) H13C(0.043) H18(0.044) H14A(0.049) H14B(0.049) H14C(0.049)
 H32(0.045) H19(0.043)
 Fixed X: H2(0.6733) H4(0.6261) H25(0.9395) H26(0.876) H23(0.7383) H27(0.748)
 H29(0.6341) H21(0.4659) H1(0.487) H17(0.2397) H12A(0.8899) H12B(0.9814)
 H12C(0.8351) H24(0.8684) H20(0.2866) H15A(0.6687) H15B(0.8081) H15C(0.7271)
 H30(0.5898) H11A(0.7233) H11B(0.8158) H11C(0.6767) H33(0.3523) H31(0.4287)
 H13A(0.9769) H13B(1.0832) H13C(0.9794) H18(0.0613) H14A(0.8513) H14B(0.993)
 H14C(0.891) H32(0.3093) H19(0.084)
 Fixed Y: H2(0.5306) H4(0.3062) H25(0.1479) H26(0.1034) H23(0.4126)
 H27(0.2133) H29(0.3026) H21(0.3934) H1(0.6178) H17(0.5662) H12A(0.5975)
 H12B(0.6749) H12C(0.7018) H24(0.3027) H20(0.3046) H15A(0.6199) H15B(0.6159)
 H15C(0.5139) H30(0.2681) H11A(0.7701) H11B(0.791) H11C(0.7478) H33(0.5156)
 H31(0.3579) H13A(0.3533) H13B(0.4396) H13C(0.4371) H18(0.4766) H14A(0.3767)
 H14B(0.3845) H14C(0.3182) H32(0.4806) H19(0.3461)
 Fixed Z: H2(0.6074) H4(0.751) H25(0.5628) H26(0.665) H23(0.5521) H27(0.7119)
 H29(0.8606) H21(0.5406) H1(0.6113) H17(0.633) H12A(0.6442) H12B(0.6947)
 H12C(0.6663) H24(0.5063) H20(0.4782) H15A(0.8979) H15B(0.9472) H15C(0.9295)
 H30(0.9691) H11A(0.744) H11B(0.8185) H11C(0.8132) H33(0.8215) H31(1.0046)
 H13A(0.7463) H13B(0.7605) H13C(0.6882) H18(0.5705) H14A(0.913) H14B(0.9042)
 H14C(0.8507) H32(0.9302) H19(0.4929)
;
_shelx_res_checksum              8849
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'