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_7039077
_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         'C39 H36 B Fe O2 P, C6 H12 O3'
_chemical_formula_sum            'C45 H48 B Fe O5 P'
_chemical_formula_weight         766.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                99.662(3)
_cell_angle_beta                 105.624(3)
_cell_angle_gamma                108.818(3)
_cell_formula_units_Z            2
_cell_length_a                   11.4433(3)
_cell_length_b                   12.5938(3)
_cell_length_c                   15.2161(5)
_cell_measurement_reflns_used    10515
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.4820
_cell_measurement_theta_min      4.3150
_cell_volume                     1919.34(12)
_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    'SIR2004 (Burla et al., 2007)'
_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 0.990
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details
;
  1 omega  -98.00   -4.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7064  125.0000  -90.0000 94

  2 omega   14.00  112.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.7064   37.0000 -150.0000 98

  3 omega  -32.00   67.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.7064  -37.0000   30.0000 99

  4 omega   23.00  109.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000  150.0000 86

  5 omega   40.00   66.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000   30.0000 26

  6 omega   32.00   77.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000 -150.0000 45

  7 omega   32.00   77.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000  120.0000 45

  8 omega   34.00   73.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000  -60.0000 39

  9 omega   26.00  145.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800    0.0000   30.0000 119

 10 omega   25.00  109.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000 -120.0000 84

 11 omega   37.00  120.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -125.0000  150.0000 83

 12 omega   79.00  158.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   30.0000   60.0000 79

 13 omega   33.00   64.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  150.0000 31

 14 omega   28.00  135.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -77.0000  -60.0000 107

 15 omega -115.00  -11.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7064  -57.0000   90.0000 104

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

 17 omega   11.00  106.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.7064   57.0000  -60.0000 95
;
_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      -0.0151853000
_diffrn_orient_matrix_UB_12      0.0581064000
_diffrn_orient_matrix_UB_13      0.0914716000
_diffrn_orient_matrix_UB_21      -0.1507522000
_diffrn_orient_matrix_UB_22      -0.0623756000
_diffrn_orient_matrix_UB_23      -0.0458637000
_diffrn_orient_matrix_UB_31      0.0059049000
_diffrn_orient_matrix_UB_32      -0.1041587000
_diffrn_orient_matrix_UB_33      0.0389599000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14467
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         73.576
_diffrn_reflns_theta_min         3.862
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.910
_exptl_absorpt_correction_T_max  0.295
_exptl_absorpt_correction_T_min  0.081
_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 light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.3822
_exptl_crystal_size_mid          0.346
_exptl_crystal_size_min          0.1804
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         7380
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0534P)^2^+0.3940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7176
_reflns_number_total             7380
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00336b2.cif
_cod_data_source_block           cmh032_ap
_cod_depositor_comments
'Adding full bibliography for 7039074--7039080.cif.'
_cod_original_cell_volume        1919.32(11)
_cod_database_code               7039077
_chemical_oxdiff_formula         C60H20FeBPO2
_chemical_oxdiff_usercomment     Hexan-Fraktion
_reflns_odcompleteness_completeness 99.01
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H4(0.028) H2(0.028) H11A(0.059) H11B(0.059) H11C(0.059)
 H12A(0.059) H12B(0.059) H12C(0.059) H13A(0.047) H13B(0.047) H13C(0.047)
 H14A(0.048) H14B(0.048) H14C(0.048) H15A(0.054) H15B(0.054) H15C(0.054)
 H17(0.036) H18(0.04) H19(0.044) H20(0.043) H21(0.035) H23(0.034) H24(0.038)
 H25(0.044) H26(0.044) H27(0.036) H29(0.033) H30(0.038) H31(0.042) H32(0.042)
 H33(0.036) H35(0.045) H36(0.041) H37(0.037) H38(0.039) H40A(0.05) H40B(0.05)
 H41A(0.05) H41B(0.05) H42A(0.046) H42B(0.046) H43A(0.05) H43B(0.05)
 H44A(0.044) H44B(0.044) H45A(0.05) H45B(0.05)
 Fixed X: H4(0.1921) H2(0.2285) H11A(-0.1498) H11B(-0.2631) H11C(-0.124) H12A(-
 0.0942) H12B(-0.2421) H12C(-0.1456) H13A(-0.0131) H13B(-0.1631) H13C(-0.0572)
 H14A(0.0075) H14B(-0.1141) H14C(0.0229) H15A(-0.0847) H15B(-0.1929) H15C(-
 0.0438) H17(0.0956) H18(0.0373) H19(0.0393) H20(0.1024) H21(0.1644)
 H23(0.1772) H24(0.1944) H25(0.2653) H26(0.3278) H27(0.3186) H29(0.4966)
 H30(0.7107) H31(0.7892) H32(0.6506) H33(0.4363) H35(0.1336) H36(0.2157)
 H37(0.3747) H38(0.4598) H40A(0.4975) H40B(0.3784) H41A(0.402) H41B(0.5145)
 H42A(0.6574) H42B(0.5498) H43A(0.6617) H43B(0.5323) H44A(0.5596) H44B(0.4241)
 H45A(0.4004) H45B(0.5288)
 Fixed Y: H4(0.6403) H2(0.8902) H11A(0.3856) H11B(0.3911) H11C(0.4155)
 H12A(0.584) H12B(0.5264) H12C(0.4647) H13A(0.8865) H13B(0.8168) H13C(0.7852)
 H14A(0.8719) H14B(0.883) H14C(0.928) H15A(0.5613) H15B(0.6139) H15C(0.6961)
 H17(0.4682) H18(0.2747) H19(0.1393) H20(0.1997) H21(0.3935) H23(0.7523)
 H24(0.8846) H25(1.0824) H26(1.1468) H27(1.0159) H29(0.9149) H30(0.9312)
 H31(0.8056) H32(0.6598) H33(0.6419) H35(0.9783) H36(1.0024) H37(0.9355)
 H38(0.8414) H40A(0.2639) H40B(0.2835) H41A(0.4533) H41B(0.4482) H42A(0.6273)
 H42B(0.6387) H43A(0.6761) H43B(0.5649) H44A(0.7985) H44B(0.6914) H45A(0.7069)
 H45B(0.8217)
 Fixed Z: H4(0.1889) H2(0.4149) H11A(0.2141) H11B(0.2517) H11C(0.3236)
 H12A(0.0655) H12B(0.0565) H12C(0.0892) H13A(0.2094) H13B(0.1504) H13C(0.117)
 H14A(0.456) H14B(0.3865) H14C(0.3732) H15A(0.4568) H15B(0.4467) H15C(0.4965)
 H17(0.1185) H18(0.0418) H19(0.1275) H20(0.2911) H21(0.3689) H23(0.1094)
 H24(0.0206) H25(0.094) H26(0.2574) H27(0.3473) H29(0.4232) H30(0.4453)
 H31(0.5142) H32(0.5565) H33(0.5329) H35(0.7149) H36(0.8783) H37(0.9414)
 H38(0.844) H40A(0.7273) H40B(0.7497) H41A(0.7115) H41B(0.6725) H42A(0.7929)
 H42B(0.7105) H43A(0.9477) H43B(0.9229) H44A(0.9932) H44B(0.96) H45A(1.1059)
 H45B(1.154)
;
_shelx_res_checksum              42691
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'