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_4085334
_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 H32 Fe P, C10 H15'
_chemical_formula_sum            'C43 H47 Fe P'
_chemical_formula_weight         650.63
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8914(2)
_cell_length_b                   14.3870(2)
_cell_length_c                   14.8324(2)
_cell_measurement_reflns_used    4205
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      73.5100
_cell_measurement_theta_min      4.0550
_cell_volume                     3391.13(8)
_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  'XL (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 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details
;
  1 omega -102.00   20.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064    0.0000  -90.0000 122

  2 omega   41.00   73.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000 -180.0000 32

  3 omega   29.00   61.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000   30.0000 32

  4 omega   31.00   59.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000 -150.0000 28

  5 omega   78.00  158.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  125.0000  120.0000 80

  6 omega   73.00  143.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  125.0000  -30.0000 70

  7 omega   34.00   64.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000   60.0000 30

  8 omega -117.00  -75.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -37.0000 -150.0000 42

  9 omega -115.00  -12.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -57.0000  120.0000 103
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0600419000
_diffrn_orient_matrix_UB_12      0.0406599000
_diffrn_orient_matrix_UB_13      -0.0713521000
_diffrn_orient_matrix_UB_21      -0.0201959000
_diffrn_orient_matrix_UB_22      -0.0989626000
_diffrn_orient_matrix_UB_23      -0.0333636000
_diffrn_orient_matrix_UB_31      -0.0732812000
_diffrn_orient_matrix_UB_32      -0.0059657000
_diffrn_orient_matrix_UB_33      0.0677174000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9730
_diffrn_reflns_theta_full        73.71
_diffrn_reflns_theta_max         73.71
_diffrn_reflns_theta_min         4.08
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.220
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72782
_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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.813
_refine_diff_density_min         -1.611
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3440
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0827
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1302P)^2^+12.6059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2229
_refine_ls_wR_factor_ref         0.2330
_reflns_number_gt                2970
_reflns_number_total             3440
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om501161y_si_002.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 4085329--4085336.cif.'
_cod_database_code               4085334
_chemical_oxdiff_formula         'C38 H62 Fe P'
_reflns_odcompleteness_completeness 98.77
_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. Uiso/Uaniso restraints and constraints
Uanis(C26) = Uanis(C27) = Uanis(C28) = Uanis(C29) = Uanis(C30)
Uanis(C21) = Uanis(C22) = Uanis(C23) = Uanis(C24) = Uanis(C25)
3. Others
 Fixed Sof: H9A(0.5) H9B(0.5) H9C(0.5) P1(0.5) C21(0.5) C22(0.5) C23(0.5)
 C24(0.5) C25(0.5) C26(0.5) H26A(0.5) H26B(0.5) H26C(0.5) C27(0.5) H27A(0.5)
 H27B(0.5) H27C(0.5) C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) C29(0.5) H29A(0.5)
 H29B(0.5) H29C(0.5) C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C101(0.5) H101(0.5)
4.a :
 C21(C22,C23,C24,C25,C26,C27,C28,C29,C30,C101,Fe1)
4.b Me refined with riding coordinates:
 C9(H9A,H9B,H9C)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18),
 C19(H19), C101(H101)
4.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C),
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_olex2_submission_original_sample_id Bab384
_olex2_submission_special_instructions 'No special instructions were received'