Synthesis, Structure, and Reactivity of Pentamethylcyclopentadienyl 2,4,6-Triphenylphosphinine Iron Complexes
Rezaei Rad, Babak; Chakraborty, Uttam; Mühldorf, Bernd; Sklorz, Julian A. W.; Bodensteiner, Michael; Müller, Christian; Wolf, Robert; Organometallics 34 (2015) 622–; doi:10.1021/om501161y

data_4085336
_publ_section_title
;
 Synthesis, Structure, and Reactivity of Pentamethylcyclopentadienyl
 2,4,6-Triphenylphosphinine Iron Complexes
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              622
_journal_paper_doi               10.1021/om501161y
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C62 H73 Fe Ga I N2 P'
_chemical_formula_sum            'C62 H74 Fe Ga I N2 P'
_chemical_formula_weight         1130.67
_chemical_name_systematic
;
 ?
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-08-26
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.0660(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.0120(2)
_cell_length_b                   13.62960(10)
_cell_length_c                   19.42900(10)
_cell_measurement_reflns_used    93206
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      76.4680
_cell_measurement_theta_min      3.8950
_cell_volume                     5295.92(7)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-1997 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(1)
_diffrn_detector_area_resol_mean 10.3546
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega -110.00  -19.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -37.0000    0.0000 91

  2 omega  -63.00   35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064   37.0000 -180.0000 98

  3 omega   15.00  117.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   37.0000  -90.0000 102

  4 omega -114.00   -7.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  111.0000  -60.0000 107

  5 omega   35.00   72.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000 -180.0000 37

  6 omega   35.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   30.0000 34

  7 omega   83.00  157.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000    0.0000 74

  8 omega   25.00  157.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000    0.0000    0.0000 132

  9 omega   29.00  109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000  -30.0000 80

 10 omega   38.00  116.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000  -60.0000 78

 11 omega   38.00  144.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000   60.0000 106

 12 omega   83.00  116.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000 -180.0000 33

 13 omega   83.00  157.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000 -150.0000 74

 14 omega   35.00  116.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000   60.0000 81

 15 omega   35.00   67.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000    0.0000 32

 16 omega   44.00  108.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000 -150.0000 64

 17 omega   38.00   64.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000 -150.0000 26

 18 omega   45.00   75.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000 -120.0000 30

 19 omega   83.00  155.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  120.0000 72

 20 omega   38.00   77.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000 -180.0000 39

 21 omega -115.00  -12.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -57.0000  120.0000 103

 22 omega    2.00   28.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   92.0000  -80.2237 26

 23 omega  -35.00   67.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064  -37.0000  -30.0000 102

 24 omega -161.00  -50.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -76.0000   79.2888 111

 25 omega -160.00  -50.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -73.0000 -162.5840 110

 26 omega -160.00  -50.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -73.0000  132.8558 110

 27 omega -160.00  -50.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -74.0000  -25.5935 110

 28 omega -162.00  -49.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -77.0000  -90.0000 113

 29 omega   29.00  109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000   30.0000 80

 30 omega   83.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  -60.0000 75

 31 omega   38.00   77.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000   60.0000 39

 32 omega   83.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000   30.0000 75

 33 omega   35.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -60.0000 34

 34 omega   35.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  120.0000 34

 35 omega   82.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000   90.0000 76

 36 omega -115.00  -12.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -57.0000  -60.0000 103

 37 omega    8.00  120.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   77.0000   90.0000 112

 38 omega    2.00   28.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   92.0000  174.6405 26

 39 omega -162.00  -49.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -77.0000   30.0000 113

 40 omega   83.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000 -150.0000 75

 41 omega   83.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  150.0000 75

 42 omega   83.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000 -120.0000 75

 43 omega   83.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  -90.0000 75

 44 omega   35.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -120.0000 34

 45 omega   83.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  -30.0000 75

 46 omega   84.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   56.0000   96.0000 74

 47 omega   35.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -150.0000 34

 48 omega   35.00  116.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000  150.0000 81

 49 omega   38.00   77.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -60.0000 39

 50 omega   35.00  116.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000 -120.0000 81

 51 omega  -98.00   -2.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  125.0000  120.0000 96

 52 omega -120.00   -8.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -77.0000 -120.0000 112

 53 omega    8.00  120.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   77.0000   30.0000 112

 54 omega -162.00 -137.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -77.0000   60.0000 25

 55 omega -162.00  -49.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -77.0000 -120.0000 113

 56 omega -162.00  -49.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -77.0000  -60.0000 113

 57 omega -161.00  -50.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -76.0000  109.3418 111

 58 omega -160.00  -50.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -73.0000    1.4855 110

 59 omega -160.00  -50.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -74.0000  163.1615 110

 60 omega   79.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  -30.0000 79

 61 omega   83.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000   60.0000 75

 62 omega   83.00  158.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000 -180.0000 75

 63 omega   29.00  109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000 -120.0000 80

 64 omega   38.00   77.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000    0.0000 39
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0471190000
_diffrn_orient_matrix_UB_12      0.0844938000
_diffrn_orient_matrix_UB_13      -0.0223092000
_diffrn_orient_matrix_UB_21      -0.0218023000
_diffrn_orient_matrix_UB_22      0.0112399000
_diffrn_orient_matrix_UB_23      0.0748372000
_diffrn_orient_matrix_UB_31      0.0569176000
_diffrn_orient_matrix_UB_32      0.0742202000
_diffrn_orient_matrix_UB_33      0.0140425000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            157209
_diffrn_reflns_theta_full        26.67
_diffrn_reflns_theta_max         26.67
_diffrn_reflns_theta_min         1.81
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.437
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2340
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.687
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         11145
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+17.6988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0921
_reflns_number_gt                10924
_reflns_number_total             11145
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om501161y_si_002.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 4085329--4085336.cif.'
_cod_database_code               4085336
_chemical_oxdiff_formula         'C72 H91 Fe P Ga'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.017) H4(0.016) H11A(0.053) H11B(0.053) H11C(0.053)
 H12A(0.051) H12B(0.051) H12C(0.051) H13A(0.038) H13B(0.038) H13C(0.038)
 H14A(0.036) H14B(0.036) H14C(0.036) H15A(0.048) H15B(0.048) H15C(0.048)
 H17(0.025) H18(0.033) H19(0.034) H20(0.034) H21(0.028) H23(0.029) H24(0.035)
 H25(0.033) H26(0.033) H27(0.025) H29(0.024) H30(0.032) H31(0.038) H32(0.037)
 H33(0.026) H37A(0.036) H37B(0.036) H37C(0.036) H38A(0.034) H38B(0.034)
 H38C(0.034) H41(0.032) H42(0.034) H43(0.029) H45(0.031) H46A(0.062)
 H46B(0.062) H46C(0.062) H47A(0.051) H47B(0.051) H47C(0.051) H48(0.025)
 H49A(0.043) H49B(0.043) H49C(0.043) H50A(0.049) H50B(0.049) H50C(0.049)
 H53(0.029) H54(0.033) H55(0.031) H57(0.024) H58A(0.044) H58B(0.044)
 H58C(0.044) H59A(0.045) H59B(0.045) H59C(0.045) H60(0.029) H61A(0.05)
 H61B(0.05) H61C(0.05) H62A(0.059) H62B(0.059) H62C(0.059)
 Fixed X: H2(0.6491) H4(0.8463) H11A(0.6048) H11B(0.5744) H11C(0.5727)
 H12A(0.6395) H12B(0.5954) H12C(0.5907) H13A(0.7455) H13B(0.7987) H13C(0.8117)
 H14A(0.8609) H14B(0.8763) H14C(0.8609) H15A(0.7846) H15B(0.7153) H15C(0.7195)
 H17(0.6181) H18(0.5092) H19(0.4232) H20(0.4467) H21(0.5547) H23(0.6647)
 H24(0.6805) H25(0.7841) H26(0.8721) H27(0.8568) H29(0.9304) H30(1.0166)
 H31(0.9981) H32(0.8939) H33(0.8069) H37A(0.9402) H37B(0.9006) H37C(0.9093)
 H38A(0.6188) H38B(0.663) H38C(0.6723) H41(0.5334) H42(0.4523) H43(0.4796)
 H45(0.7077) H46A(0.6924) H46B(0.665) H46C(0.6153) H47A(0.6915) H47B(0.6147)
 H47C(0.6659) H48(0.6394) H49A(0.5908) H49B(0.5358) H49C(0.6107) H50A(0.5602)
 H50B(0.5593) H50C(0.5033) H53(1.0468) H54(1.0589) H55(0.9721) H57(0.9079)
 H58A(0.9414) H58B(0.9049) H58C(0.9831) H59A(1.0033) H59B(1.0491) H59C(1.0091)
 H60(0.8087) H61A(0.8146) H61B(0.8455) H61C(0.8925) H62A(0.8159) H62B(0.8938)
 H62C(0.8481)
 Fixed Y: H2(0.9941) H4(1.0128) H11A(1.0531) H11B(1.1505) H11C(1.0543)
 H12A(1.2465) H12B(1.1556) H12C(1.2523) H13A(1.2779) H13B(1.3116) H13C(1.2177)
 H14A(1.1214) H14B(1.1343) H14C(1.2264) H15A(1.0486) H15B(1.0892) H15C(0.9867)
 H17(0.8151) H18(0.8003) H19(0.8787) H20(0.9665) H21(0.9797) H23(1.1194)
 H24(1.2159) H25(1.2232) H26(1.1321) H27(1.0364) H29(0.9677) H30(0.967)
 H31(0.9164) H32(0.8583) H33(0.8584) H37A(0.5333) H37B(0.434) H37C(0.4926)
 H38A(0.4777) H38B(0.4498) H38C(0.3939) H41(0.5802) H42(0.6427) H43(0.6929)
 H45(0.5658) H46A(0.5584) H46B(0.6581) H46C(0.5736) H47A(0.4105) H47B(0.4176)
 H47C(0.412) H48(0.6734) H49A(0.815) H49B(0.8143) H49C(0.834) H50A(0.6493)
 H50B(0.5605) H50C(0.6408) H53(0.7652) H54(0.716) H55(0.6381) H57(0.7181)
 H58A(0.8777) H58B(0.8795) H58C(0.8864) H59A(0.7315) H59B(0.734) H59C(0.6386)
 H60(0.6104) H61A(0.4449) H61B(0.4632) H61C(0.4471) H62A(0.5687) H62B(0.5796)
 H62C(0.6719)
 Fixed Z: H2(-0.0094) H4(-0.044) H11A(-0.2602) H11B(-0.232) H11C(-0.1878)
 H12A(-0.043) H12B(-0.0643) H12C(-0.1079) H13A(-0.0308) H13B(-0.0831) H13C(-
 0.0379) H14A(-0.2264) H14B(-0.1472) H14C(-0.1934) H15A(-0.2925) H15B(-0.3198)
 H15C(-0.2833) H17(-0.2007) H18(-0.242) H19(-0.1881) H20(-0.088) H21(-0.0446)
 H23(0.054) H24(0.1504) H25(0.2067) H26(0.1657) H27(0.0682) H29(-0.0951) H30(-
 0.1708) H31(-0.2832) H32(-0.3186) H33(-0.2435) H37A(0.0005) H37B(-0.0013)
 H37C(0.0679) H38A(0.0099) H38B(0.0753) H38C(0.0057) H41(-0.1921) H42(-0.1233)
 H43(-0.0127) H45(-0.1506) H46A(-0.2702) H46B(-0.2425) H46C(-0.2635) H47A(-
 0.2004) H47B(-0.1879) H47C(-0.1251) H48(0.0731) H49A(0.1193) H49B(0.0598)
 H49C(0.0431) H50A(0.1577) H50B(0.1063) H50C(0.1004) H53(-0.0441) H54(-0.1561)
 H55(-0.2149) H57(0.0604) H58A(0.0933) H58B(0.0205) H58C(0.0268) H59A(0.134)
 H59B(0.0702) H59C(0.0871) H60(-0.1614) H61A(-0.19) H61B(-0.1158) H61C(-0.1777)
 H62A(-0.2777) H62B(-0.2721) H62C(-0.2637)
;
_olex2_submission_special_instructions 'No special instructions were received'