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_7039079
_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         'C36 H41 Fe P Si'
_chemical_formula_sum            'C36 H41 Fe P Si'
_chemical_formula_weight         588.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6876(2)
_cell_length_b                   16.4330(3)
_cell_length_c                   17.8191(3)
_cell_measurement_reflns_used    5627
_cell_measurement_temperature    122.8(6)
_cell_measurement_theta_max      66.2730
_cell_measurement_theta_min      4.9230
_cell_volume                     3129.56(10)
_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 0.992
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega  -31.00   70.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4087  -57.0000  -30.0000 101

  2 omega   33.00  159.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000  -60.0000 126

  3 omega   32.00   89.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000 -150.0000 57

  4 omega   16.00   75.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000 -150.0000 59

  5 omega   20.00   70.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -90.0000 50

  6 omega   24.00   67.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000  150.0000 43

  7 omega  -83.00  -39.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4087  125.0000 -180.0000 44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0452378000
_diffrn_orient_matrix_UB_12      -0.0703640000
_diffrn_orient_matrix_UB_13      -0.0502449000
_diffrn_orient_matrix_UB_21      -0.0483450000
_diffrn_orient_matrix_UB_22      -0.0619335000
_diffrn_orient_matrix_UB_23      0.0580401000
_diffrn_orient_matrix_UB_31      -0.1280950000
_diffrn_orient_matrix_UB_32      -0.0016076000
_diffrn_orient_matrix_UB_33      -0.0396948000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9232
_diffrn_reflns_point_group_measured_fraction_full 0.910
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.827
_diffrn_reflns_theta_min         4.825
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.871
_exptl_absorpt_correction_T_max  0.763
_exptl_absorpt_correction_T_min  0.627
_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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.5012
_exptl_crystal_size_mid          0.4774
_exptl_crystal_size_min          0.3237
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 1736 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0600P)^2^+0.5716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1001
_reflns_Friedel_coverage         0.626
_reflns_Friedel_fraction_full    0.805
_reflns_Friedel_fraction_max     0.798
_reflns_number_gt                4852
_reflns_number_total             5039
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00336b2.cif
_cod_data_source_block           cmh027_red
_cod_depositor_comments
'Adding full bibliography for 7039074--7039080.cif.'
_cod_original_cell_volume        3129.54(10)
_cod_database_code               7039079
_chemical_oxdiff_formula         C36H41FePSi
_reflns_odcompleteness_completeness 98.40
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.024) H4(0.026) H11A(0.076) H11B(0.076) H11C(0.076)
 H12A(0.086) H12B(0.086) H12C(0.086) H13A(0.078) H13B(0.078) H13C(0.078)
 H14A(0.056) H14B(0.056) H14C(0.056) H15A(0.062) H15B(0.062) H15C(0.062)
 H17(0.034) H18(0.041) H19(0.038) H20(0.038) H21(0.032) H23(0.038) H24(0.048)
 H25(0.047) H26(0.044) H27(0.035) H29(0.032) H30(0.041) H31(0.043) H32(0.039)
 H33(0.031) H34A(0.047) H34B(0.047) H34C(0.047) H35A(0.061) H35B(0.061)
 H35C(0.061) H36A(0.054) H36B(0.054) H36C(0.054)
 Fixed X: H2(0.6173) H4(0.683) H11A(0.822) H11B(0.9552) H11C(0.8367)
 H12A(0.8434) H12B(0.9549) H12C(0.8177) H13A(0.9353) H13B(1.0172) H13C(0.8723)
 H14A(0.9213) H14B(1.0537) H14C(0.9422) H15A(0.8783) H15B(1.019) H15C(0.9171)
 H17(0.5839) H18(0.5552) H19(0.5181) H20(0.5141) H21(0.5445) H23(0.5258)
 H24(0.5457) H25(0.6654) H26(0.7623) H27(0.7433) H29(0.7103) H30(0.7745)
 H31(0.7719) H32(0.6974) H33(0.6302) H34A(0.3509) H34B(0.2208) H34C(0.3423)
 H35A(0.2312) H35B(0.154) H35C(0.2766) H36A(0.3344) H36B(0.1963) H36C(0.2899)
 Fixed Y: H2(0.4159) H4(0.1736) H11A(0.4152) H11B(0.3812) H11C(0.3262)
 H12A(0.4903) H12B(0.5008) H12C(0.4929) H13A(0.3123) H13B(0.3854) H13C(0.3961)
 H14A(0.131) H14B(0.1679) H14C(0.1844) H15A(0.193) H15B(0.187) H15C(0.136)
 H17(0.3741) H18(0.4872) H19(0.613) H20(0.6237) H21(0.5111) H23(0.4072)
 H24(0.4323) H25(0.348) H26(0.2355) H27(0.2099) H29(0.0604) H30(-0.062) H31(-
 0.0853) H32(0.0153) H33(0.1377) H34A(0.3111) H34B(0.2673) H34C(0.2169)
 H35A(0.3082) H35B(0.3262) H35C(0.3753) H36A(0.1008) H36B(0.1302) H36C(0.1291)
 Fixed Z: H2(0.7279) H4(0.699) H11A(0.9408) H11B(0.9604) H11C(0.9713)
 H12A(0.7425) H12B(0.7988) H12C(0.8291) H13A(0.6214) H13B(0.6493) H13C(0.6398)
 H14A(0.7389) H14B(0.7222) H14C(0.6671) H15A(0.9369) H15B(0.9126) H15C(0.8703)
 H17(0.9732) H18(1.0474) H19(0.9927) H20(0.8645) H21(0.7895) H23(0.6127)
 H24(0.4858) H25(0.4114) H26(0.4639) H27(0.591) H29(0.7385) H30(0.7874)
 H31(0.9142) H32(0.9947) H33(0.9467) H34A(0.7046) H34B(0.7084) H34C(0.692)
 H35A(0.9266) H35B(0.8537) H35C(0.8704) H36A(0.8187) H36B(0.8306) H36C(0.8983)
;
_shelx_res_checksum              41094
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'