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_4085335
_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         'C33 H33 Fe P'
_chemical_formula_sum            'C33 H33 Fe P'
_chemical_formula_weight         516.41
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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
_cell_angle_beta                 106.8577(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9388(2)
_cell_length_b                   16.8436(2)
_cell_length_c                   13.23897(18)
_cell_measurement_reflns_used    9338
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      75.8430
_cell_measurement_theta_min      4.3290
_cell_volume                     2547.85(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
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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)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector_area_resol_mean 10.3546
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
  1 omega  -67.00   28.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064   37.0000  120.0000 95

  2 omega  -33.00   71.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064  -57.0000 -180.0000 104

  3 omega   37.00   68.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -90.0000 31

  4 omega   43.00   69.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -120.0000 26

  5 omega   36.00   69.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   60.0000 33

  6 omega   39.00  143.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -61.0000   30.0000 104

  7 omega   39.00   68.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -60.0000 29

  8 omega   39.00   69.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -30.0000 30

  9 omega   35.00   68.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   30.0000 33

 10 omega  113.00  149.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000   30.0000 36

 11 omega   38.00   69.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -180.0000 31

 12 omega   29.00  106.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -94.0000  -60.0000 77

 13 omega   30.00  137.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000    0.0000 -150.0000 107

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

 15 omega -115.00  -12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -57.0000 -150.0000 103

 16 omega -115.00  -12.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -57.0000  -30.0000 103

 17 omega -162.00  -71.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -77.0000 -180.0000 91

 18 omega   35.00  116.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -111.0000 -120.0000 81

 19 omega   83.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000   60.0000 75

 20 omega   82.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000  -90.0000 76

 21 omega   83.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  -60.0000 75

 22 omega   85.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000 -150.0000 73

 23 omega   85.00  158.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000    0.0000 73
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0226310000
_diffrn_orient_matrix_UB_12      -0.0064166000
_diffrn_orient_matrix_UB_13      -0.1204033000
_diffrn_orient_matrix_UB_21      0.0805665000
_diffrn_orient_matrix_UB_22      0.0719187000
_diffrn_orient_matrix_UB_23      0.0026589000
_diffrn_orient_matrix_UB_31      0.1055453000
_diffrn_orient_matrix_UB_32      -0.0562383000
_diffrn_orient_matrix_UB_33      0.0170721000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23025
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.664
_diffrn_reflns_theta_min         4.367
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.474
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73599
_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    1.346
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.1086
_exptl_crystal_size_min          0.0482
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         5281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0643P)^2^+1.4578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4649
_reflns_number_total             5281
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501161y_si_002.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 4085329--4085336.cif.'
_cod_original_cell_volume        2547.84(7)
_cod_database_code               4085335
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C132 H132 Fe P'
_reflns_odcompleteness_completeness 99.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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 Me refined with riding coordinates:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36), C52(H52), C53(H53), C54(H54), C55(H55),
  C56(H56)
;
_shelx_res_checksum              96476
_shelx_hkl_checksum              46059
_olex2_submission_special_instructions 'No special instructions were received'