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_7039076
_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         'C51 H47 Fe P Sn'
_chemical_formula_sum            'C51 H47 Fe P Sn'
_chemical_formula_weight         865.39
_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                 105.5303(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.87702(14)
_cell_length_b                   20.79053(20)
_cell_length_c                   14.68647(16)
_cell_measurement_reflns_used    16595
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.3640
_cell_measurement_theta_min      3.8800
_cell_volume                     4082.50(8)
_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 0.995
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
  1 omega -112.00  -12.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7064  -57.0000 -150.0000 100

  2 omega  -65.00   21.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7064   57.0000  150.0000 86

  3 omega   29.00   66.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  -90.0000 37

  4 omega   34.00  121.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -125.0000  -30.0000 87

  5 omega   32.00  110.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -125.0000  120.0000 78

  6 omega   34.00  134.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -61.0000  120.0000 100

  7 omega   33.00   68.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  -60.0000 35

  8 omega   84.00  158.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   30.0000   60.0000 74

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

 10 omega -117.00  -14.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7064  -37.0000   90.0000 103

 11 omega   46.00  158.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   15.0000  -60.0000 112

 12 omega   79.00  158.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000  120.0000 79

 13 omega   77.00  125.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000 -180.0000 48
;
_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      0.0040258000
_diffrn_orient_matrix_UB_12      -0.0739698000
_diffrn_orient_matrix_UB_13      -0.0050423000
_diffrn_orient_matrix_UB_21      0.0981811000
_diffrn_orient_matrix_UB_22      -0.0000845000
_diffrn_orient_matrix_UB_23      0.0797799000
_diffrn_orient_matrix_UB_31      -0.0601996000
_diffrn_orient_matrix_UB_32      -0.0050786000
_diffrn_orient_matrix_UB_33      0.0738309000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24280
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         73.441
_diffrn_reflns_theta_min         3.779
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.338
_exptl_absorpt_correction_T_max  0.797
_exptl_absorpt_correction_T_min  0.571
_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 red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       plank
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.4394
_exptl_crystal_size_mid          0.2624
_exptl_crystal_size_min          0.1316
_refine_diff_density_max         1.403
_refine_diff_density_min         -1.285
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         7980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0531P)^2^+3.5028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0912
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7601
_reflns_number_total             7980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00336b2.cif
_cod_data_source_block           cmh048_mp
_cod_depositor_comments
'Adding full bibliography for 7039074--7039080.cif.'
_cod_database_code               7039076
_chemical_oxdiff_formula         C51H47FePSn
_chemical_oxdiff_usercomment     Hexan-Fraktion
_reflns_odcompleteness_completeness 99.38
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.021) H4(0.022) H11A(0.103) H11B(0.103) H11C(0.103)
 H12A(0.086) H12B(0.086) H12C(0.086) H13A(0.082) H13B(0.082) H13C(0.082)
 H14A(0.086) H14B(0.086) H14C(0.086) H15A(0.098) H15B(0.098) H15C(0.098)
 H17(0.025) H18(0.03) H19(0.035) H20(0.038) H21(0.03) H23(0.031) H24(0.039)
 H25(0.041) H26(0.037) H27(0.031) H29(0.026) H30(0.029) H31(0.032) H32(0.032)
 H33(0.027) H35(0.038) H36(0.053) H37(0.056) H38(0.048) H39(0.035) H41(0.025)
 H42(0.032) H43(0.036) H44(0.037) H45(0.03) H47(0.031) H48(0.041) H49(0.044)
 H50(0.044) H51(0.037)
 Fixed X: H2(0.6423) H4(0.8793) H11A(0.4329) H11B(0.4525) H11C(0.491)
 H12A(0.5436) H12B(0.4758) H12C(0.4682) H13A(0.8067) H13B(0.7081) H13C(0.72)
 H14A(0.8702) H14B(0.8407) H14C(0.883) H15A(0.6432) H15B(0.6619) H15C(0.7517)
 H17(0.4493) H18(0.283) H19(0.2312) H20(0.3445) H21(0.5111) H23(0.7628)
 H24(0.8641) H25(1.0022) H26(1.0386) H27(0.9383) H29(0.9337) H30(0.9935)
 H31(0.9045) H32(0.7555) H33(0.6942) H35(0.6992) H36(0.5707) H37(0.4065)
 H38(0.3697) H39(0.4961) H41(0.8089) H42(0.948) H43(1.0839) H44(1.0803)
 H45(0.9417) H47(0.7125) H48(0.7601) H49(0.858) H50(0.9079) H51(0.8589)
 Fixed Y: H2(0.5951) H4(0.5623) H11A(0.602) H11B(0.6276) H11C(0.5593)
 H12A(0.7029) H12B(0.7263) H12C(0.6552) H13A(0.742) H13B(0.7828) H13C(0.7281)
 H14A(0.6418) H14B(0.7135) H14C(0.6936) H15A(0.5587) H15B(0.6264) H15C(0.5871)
 H17(0.4776) H18(0.4682) H19(0.5037) H20(0.5503) H21(0.5604) H23(0.5963)
 H24(0.6561) H25(0.7097) H26(0.7034) H27(0.6438) H29(0.5362) H30(0.5096)
 H31(0.4413) H32(0.397) H33(0.4242) H35(0.2842) H36(0.2401) H37(0.2646)
 H38(0.3357) H39(0.3812) H41(0.4771) H42(0.4959) H43(0.4269) H44(0.3392)
 H45(0.3211) H47(0.2247) H48(0.1384) H49(0.155) H50(0.2577) H51(0.3446)
 Fixed Z: H2(0.1706) H4(0.3977) H11A(0.3584) H11B(0.4622) H11C(0.4434)
 H12A(0.2043) H12B(0.2676) H12C(0.2311) H13A(0.339) H13B(0.3176) H13C(0.248)
 H14A(0.5496) H14B(0.561) H14C(0.4762) H15A(0.5739) H15B(0.6226) H15C(0.605)
 H17(0.3035) H18(0.2189) H19(0.064) H20(-0.0044) H21(0.078) H23(0.0886)
 H24(0.0189) H25(0.1111) H26(0.274) H27(0.3445) H29(0.532) H30(0.6893)
 H31(0.7609) H32(0.6715) H33(0.5141) H35(0.0735) H36(-0.045) H37(-0.0547)
 H38(0.0502) H39(0.1687) H41(0.1261) H42(0.0724) H43(0.1136) H44(0.2103)
 H45(0.2658) H47(0.2532) H48(0.3548) H49(0.5071) H50(0.5574) H51(0.4578)
;
_shelx_res_checksum              38083
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'