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_4085333
_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         'C35 H38 Fe N P'
_chemical_formula_sum            'C35 H38 Fe N P'
_chemical_formula_weight         559.48
_chemical_name_systematic
;
 ?
;
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2014-08-27
_audit_creation_method
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Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                102.503(2)
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_cell_formula_units_Z            8
_cell_length_a                   17.6804(5)
_cell_length_b                   18.1961(5)
_cell_length_c                   18.5988(6)
_cell_measurement_reflns_used    14617
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      73.4290
_cell_measurement_theta_min      3.4280
_cell_volume                     5718.6(3)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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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)'
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_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(1)
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_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_details
;
  1 omega -112.00  -13.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
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  2 omega    8.00  102.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   77.0000   30.0000 94

  3 omega  -16.00   82.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064  -99.0000  -90.0000 98

  4 omega   23.00  109.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000  120.0000 86

  5 omega   78.00  133.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -77.0000 -120.0000 55

  6 omega   99.00  158.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  125.0000 -180.0000 59

  7 omega   73.00  158.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000  -90.0000 85

  8 omega   23.00  109.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000   30.0000 86

  9 omega   79.00  158.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000 -120.0000 79

 10 omega   36.00   67.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -77.0000 -120.0000 31

 11 omega   23.00  109.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000 -150.0000 86

 12 omega   47.00   77.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000   90.0000 30

 13 omega   79.00  158.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000  -30.0000 79

 14 omega   77.00  158.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000 -180.0000 81

 15 omega   92.00  121.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -125.0000    0.0000 29

 16 omega   33.00   60.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -125.0000    0.0000 27

 17 omega -115.00  -12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -57.0000 -120.0000 103

 18 omega  -33.00   71.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064  -57.0000  -30.0000 104

 19 omega  -35.00   67.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064  -37.0000   90.0000 102

 20 omega   76.00  110.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   30.0000   90.0000 34
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0114475000
_diffrn_orient_matrix_UB_12      0.0277035000
_diffrn_orient_matrix_UB_13      0.0726364000
_diffrn_orient_matrix_UB_21      0.0880998000
_diffrn_orient_matrix_UB_22      -0.0093740000
_diffrn_orient_matrix_UB_23      0.0105936000
_diffrn_orient_matrix_UB_31      -0.0055890000
_diffrn_orient_matrix_UB_32      0.0836332000
_diffrn_orient_matrix_UB_33      -0.0427474000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            46955
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.162
_diffrn_reflns_theta_min         3.108
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.928
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51819
_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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description
;
;
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.1756
_exptl_crystal_size_mid          0.1492
_exptl_crystal_size_min          0.0974
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1397
_refine_ls_number_reflns         22060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0514P)^2^+1.4455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1175
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16719
_reflns_number_total             22060
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501161y_si_002.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 4085329--4085336.cif.'
_cod_database_code               4085333
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C280 H304 Fe8 N8 P8'
_reflns_odcompleteness_completeness 99.06
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C12(H12), C14(H14), C29(H29), C31(H31), C46(H46), C48(H48), C63(H63), C65(H65)
2.b Aromatic/amide H refined with riding coordinates:
 C112(H112), C113(H113), C114(H114), C115(H115), C116(H116), C132(H132),
 C133(H133), C134(H134), C135(H135), C136(H136), C152(H152), C153(H153),
 C154(H154), C155(H155), C156(H156), C282(H282), C283(H283), C284(H284),
 C285(H285), C286(H286), C302(H302), C303(H303), C304(H304), C305(H305),
 C306(H306), C322(H322), C323(H323), C324(H324), C325(H325), C326(H326),
 C452(H452), C453(H453), C454(H454), C455(H455), C456(H456), C472(H472),
 C473(H473), C474(H474), C475(H475), C476(H476), C492(H492), C493(H493),
 C494(H494), C495(H495), C496(H496), C622(H622), C623(H623), C624(H624),
 C625(H625), C626(H626), C642(H642), C643(H643), C644(H644), C645(H645),
 C646(H646), C662(H662), C663(H663), C664(H664), C665(H665), C666(H666)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C23(H23A,H23B,H23C),
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C40(H40A,H40B,H40C), C41(H41A,
 H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C),
 C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C57(H57A,H57B,H57C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C67(H67A,
 H67B,H67C), C68(H68A,H68B,H68C)
;
_shelx_res_checksum              39005
_shelx_hkl_checksum              11087
_olex2_submission_special_instructions 'No special instructions were received'