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_7039074
_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                 91.5613(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.55009(11)
_cell_length_b                   19.9687(3)
_cell_length_c                   15.16204(17)
_cell_measurement_reflns_used    8870
_cell_measurement_temperature    123.00(14)
_cell_measurement_theta_max      66.5010
_cell_measurement_theta_min      5.1530
_cell_volume                     2587.72(6)
_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 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega   16.00  107.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5337   38.0000 -120.0000 91

  2 omega   12.00   85.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5337   57.0000  -30.0000 73

  3 omega   28.00   65.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000 -150.0000 37

  4 omega   21.00   76.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000 -180.0000 55

  5 omega   82.00  113.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000 -180.0000 31

  6 omega   16.00   55.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  -60.0000 39

  7 omega   27.00   62.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000 -180.0000 35

  8 omega   26.00   55.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  -30.0000 29

  9 omega   34.00   70.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000  150.0000 36

 10 omega   79.00  119.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000   90.0000 40

 11 omega  134.00  160.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000   90.0000 26

 12 omega   69.00  155.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000   60.0000 86

 13 omega   65.00   91.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000  -90.0000 26

 14 omega  117.00  163.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000  -90.0000 46

 15 omega   35.00  126.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -92.0000 -164.2730 91

 16 omega  -99.00  -18.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5337  125.0000   30.0000 81

 17 omega    8.00  120.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5337   77.0000   90.0000 112

 18 omega   66.00  168.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000  -30.0000 102

 19 omega   63.00   89.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000 -150.0000 26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1117393000
_diffrn_orient_matrix_UB_12      0.0111027000
_diffrn_orient_matrix_UB_13      -0.0766680000
_diffrn_orient_matrix_UB_21      0.1375234000
_diffrn_orient_matrix_UB_22      0.0094647000
_diffrn_orient_matrix_UB_23      0.0666168000
_diffrn_orient_matrix_UB_31      0.0334934000
_diffrn_orient_matrix_UB_32      -0.0757461000
_diffrn_orient_matrix_UB_33      -0.0029464000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16543
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.723
_diffrn_reflns_theta_max         66.723
_diffrn_reflns_theta_min         3.661
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.390
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.851
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.326
_exptl_crystal_description       plank
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.1665
_exptl_crystal_size_mid          0.1053
_exptl_crystal_size_min          0.1052
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         4548
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0366P)^2^+2.1542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4275
_reflns_number_total             4548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00336b2.cif
_cod_data_source_block           cmh060_mp
_cod_depositor_comments
'Adding full bibliography for 7039074--7039080.cif.'
_cod_original_cell_volume        2587.71(5)
_cod_database_code               7039074
_chemical_oxdiff_formula         C33H33FeP
_chemical_oxdiff_usercomment     Hexan-Fraktion
_reflns_odcompleteness_completeness 98.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.023) H2(0.024) H4(0.02) H11A(0.042) H11B(0.042) H11C(0.042)
 H12A(0.04) H12B(0.04) H12C(0.04) H13A(0.037) H13B(0.037) H13C(0.037)
 H14A(0.036) H14B(0.036) H14C(0.036) H15A(0.037) H15B(0.037) H15C(0.037)
 H17(0.029) H18(0.037) H19(0.038) H20(0.043) H21(0.039) H23(0.027) H24(0.032)
 H25(0.033) H26(0.031) H27(0.026) H29(0.031) H30(0.039) H31(0.041) H32(0.038)
 H33(0.031)
 Fixed X: H1(0.7589) H2(0.6759) H4(0.5543) H11A(0.2543) H11B(0.0778)
 H11C(0.1802) H12A(0.4764) H12B(0.3088) H12C(0.4061) H13A(0.3943) H13B(0.3077)
 H13C(0.4781) H14A(0.1752) H14B(0.1042) H14C(0.2825) H15A(0.0829) H15B(-0.0352)
 H15C(0.1014) H17(0.8911) H18(0.9522) H19(0.8152) H20(0.6145) H21(0.5532)
 H23(0.8747) H24(0.9989) H25(0.9197) H26(0.7161) H27(0.5933) H29(0.3894)
 H30(0.2361) H31(0.1382) H32(0.1995) H33(0.3563)
 Fixed Y: H1(0.7255) H2(0.6006) H4(0.7644) H11A(0.5838) H11B(0.594)
 H11C(0.6556) H12A(0.5064) H12B(0.4789) H12C(0.5146) H13A(0.6015) H13B(0.536)
 H13C(0.5504) H14A(0.7559) H14B(0.6934) H14C(0.7102) H15A(0.7421) H15B(0.7253)
 H15C(0.7761) H17(0.714) H18(0.6568) H19(0.5618) H20(0.5245) H21(0.5804)
 H23(0.5942) H24(0.5476) H25(0.574) H26(0.6493) H27(0.6971) H29(0.8389)
 H30(0.9329) H31(0.9876) H32(0.9484) H33(0.855)
 Fixed Z: H1(0.328) H2(0.2592) H4(0.1062) H11A(0.3834) H11B(0.356)
 H11C(0.3857) H12A(0.2041) H12B(0.2225) H12C(0.2979) H13A(-0.0039) H13B(0.0242)
 H13C(0.0601) H14A(0.0584) H14B(0.0093) H14C(0.0017) H15A(0.2967) H15B(0.219)
 H15C(0.2044) H17(0.4649) H18(0.5932) H19(0.6299) H20(0.5374) H21(0.4083)
 H23(0.1646) H24(0.0464) H25(-0.0966) H26(-0.1206) H27(-0.0027) H29(0.0878)
 H30(0.0701) H31(0.1912) H32(0.3312) H33(0.3503)
;
_shelx_res_checksum              88752
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'