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_7039078
_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         'C45 H42 Fe P2'
_chemical_formula_sum            'C45 H42 Fe P2'
_chemical_formula_weight         700.57
_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                 116.708(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.8847(5)
_cell_length_b                   8.53295(15)
_cell_length_c                   22.0647(5)
_cell_measurement_reflns_used    14309
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.0300
_cell_measurement_theta_min      4.7420
_cell_volume                     3512.59(16)
_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)'
_computing_structure_solution    'ShelXT (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 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
  1 omega   15.00  117.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.7064   37.0000 -180.0000 102

  2 omega    2.00   98.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.7064 -125.0000  -60.0000 96

  3 omega   29.00   65.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000   90.0000 36

  4 omega   39.00   77.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000 -150.0000 38

  5 omega   33.00   64.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  150.0000 31

  6 omega   41.00   76.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000   60.0000 35

  7 omega   77.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000   90.0000 81

  8 omega   34.00   77.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000 -120.0000 43

  9 omega   35.00   60.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000 -180.0000 25

 10 omega   77.00  152.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000  -30.0000 75

 11 omega   92.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000   60.0000 66

 12 omega  -33.00   70.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.7064  -57.0000   30.0000 103

 13 omega    7.00  119.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.7064   77.0000   30.0000 112

 14 omega   14.00  117.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.7064   37.0000  -60.0000 103

 15 omega   73.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000  120.0000 85

 16 omega   46.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   15.0000  -90.0000 112

 17 omega   32.00   77.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000   30.0000 45

 18 omega   79.00  158.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000   30.0000 79

 19 omega   23.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000 -180.0000 86

 20 omega   32.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -125.0000   60.0000 89

 21 omega   11.00  115.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.7064   57.0000  -30.0000 104
;
_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      -0.0075349000
_diffrn_orient_matrix_UB_12      0.0422720000
_diffrn_orient_matrix_UB_13      0.0643433000
_diffrn_orient_matrix_UB_21      -0.0597162000
_diffrn_orient_matrix_UB_22      -0.1232990000
_diffrn_orient_matrix_UB_23      -0.0186969000
_diffrn_orient_matrix_UB_31      0.0566023000
_diffrn_orient_matrix_UB_32      -0.1249622000
_diffrn_orient_matrix_UB_33      0.0402008000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29448
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         73.537
_diffrn_reflns_theta_min         4.741
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.536
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.881
_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            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.1612
_exptl_crystal_size_mid          0.1289
_exptl_crystal_size_min          0.1012
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         6982
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0403P)^2^+2.2634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0876
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6537
_reflns_number_total             6982
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00336b2.cif
_cod_data_source_block           cmh063_mp
_cod_depositor_comments
'Adding full bibliography for 7039074--7039080.cif.'
_cod_original_cell_volume        3512.60(15)
_cod_database_code               7039078
_chemical_oxdiff_formula         C45H42FeP2
_chemical_oxdiff_usercomment     Et2O-Fraktion
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.026) H4(0.024) H11A(0.068) H11B(0.068) H11C(0.068)
 H12A(0.061) H12B(0.061) H12C(0.061) H13A(0.076) H13B(0.076) H13C(0.076)
 H14A(0.088) H14B(0.088) H14C(0.088) H15A(0.088) H15B(0.088) H15C(0.088)
 H17(0.033) H18(0.039) H19(0.045) H20(0.045) H21(0.036) H23(0.04) H24(0.044)
 H25(0.034) H26(0.035) H27(0.033) H29(0.038) H30(0.047) H31(0.046) H32(0.042)
 H33(0.034) H35(0.035) H36(0.043) H37(0.042) H38(0.038) H39(0.032) H41(0.033)
 H42(0.039) H43(0.042) H44(0.039) H45(0.032)
 Fixed X: H2(0.8717) H4(0.6922) H11A(0.7331) H11B(0.6894) H11C(0.6537)
 H12A(0.8998) H12B(0.8748) H12C(0.8498) H13A(0.8537) H13B(0.8759) H13C(0.9019)
 H14A(0.657) H14B(0.6945) H14C(0.737) H15A(0.5805) H15B(0.5869) H15C(0.5815)
 H17(0.7437) H18(0.8054) H19(0.923) H20(0.979) H21(0.9185) H23(0.9309)
 H24(1.0001) H25(0.9479) H26(0.8248) H27(0.7549) H29(0.5874) H30(0.4647)
 H31(0.3894) H32(0.4367) H33(0.5587) H35(0.582) H36(0.5267) H37(0.5711)
 H38(0.6713) H39(0.7267) H41(0.8005) H42(0.9217) H43(0.9909) H44(0.9365)
 H45(0.8142)
 Fixed Y: H2(0.5765) H4(0.7483) H11A(0.1267) H11B(0.0312) H11C(0.1731)
 H12A(0.2811) H12B(0.1105) H12C(0.1893) H13A(0.5202) H13B(0.3448) H13C(0.435)
 H14A(0.5481) H14B(0.4295) H14C(0.5746) H15A(0.2874) H15B(0.2316) H15C(0.4109)
 H17(0.2865) H18(0.1502) H19(0.2136) H20(0.413) H21(0.5472) H23(0.7458)
 H24(0.8909) H25(1.0305) H26(1.0242) H27(0.8778) H29(0.8393) H30(0.855)
 H31(0.6744) H32(0.483) H33(0.4682) H35(0.8649) H36(0.7508) H37(0.5218)
 H38(0.404) H39(0.5174) H41(0.7499) H42(0.7936) H43(0.8769) H44(0.9296)
 H45(0.8946)
 Fixed Z: H2(0.3542) H4(0.1983) H11A(0.333) H11B(0.2662) H11C(0.2845)
 H12A(0.3378) H12B(0.3113) H12C(0.3613) H13A(0.1838) H13B(0.1834) H13C(0.2523)
 H14A(0.0928) H14B(0.0648) H14C(0.1076) H15A(0.18) H15B(0.1153) H15C(0.1278)
 H17(0.4221) H18(0.5227) H19(0.5944) H20(0.5655) H21(0.4648) H23(0.3344)
 H24(0.2983) H25(0.1977) H26(0.1342) H27(0.1692) H29(0.1691) H30(0.1022)
 H31(0.1155) H32(0.1978) H33(0.2657) H35(0.4428) H36(0.5023) H37(0.562)
 H38(0.5621) H39(0.5027) H41(0.5606) H42(0.6242) H43(0.5729) H44(0.4573)
 H45(0.3937)
;
_shelx_res_checksum              12424
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'