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_4085332
_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         'I, C33 H32 Fe P1, C6 D6'
_chemical_formula_sum            'C39 H32 D6 Fe I P'
_chemical_formula_weight         726.50
_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   geom
_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                 98.0110(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.28930(10)
_cell_length_b                   15.26010(10)
_cell_length_c                   18.9527(2)
_cell_measurement_reflns_used    16105
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      68.5010
_cell_measurement_theta_min      3.7050
_cell_volume                     3233.23(5)
_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 (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 0.991
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
  1 omega  -91.00   -6.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  125.0000  -60.0000 85

  2 omega   20.00  113.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   37.0000 -180.0000 93

  3 omega   19.00   67.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       96.4842  -30.0000   30.0000 48

  4 omega   66.00  157.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       96.4842   61.0000  150.0000 91

  5 omega   70.00  158.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       96.4842   45.0000  -90.0000 88

  6 omega   19.00  127.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       96.4842  -77.0000    0.0000 108

  7 omega   51.00   77.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       96.4842  -45.0000  150.0000 26

  8 omega -115.00  -12.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -57.0000 -120.0000 103

  9 omega -120.00   -8.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -77.0000   30.0000 112

 10 omega  -69.00   -5.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000   30.0000  -30.0000 64

 11 omega   66.00  158.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       96.4842   30.0000   90.0000 92

 12 omega   63.00  158.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       96.4842   77.0000 -180.0000 95

 13 omega   73.00  158.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       96.4842  125.0000  -60.0000 85

 14 omega -120.00   -8.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -77.0000  150.0000 112

 15 omega  -71.00   33.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064   57.0000  150.0000 104

 16 omega -157.00  -53.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -61.0000  -30.0000 104

 17 omega   22.00  122.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       96.4842 -125.0000    0.0000 100

 18 omega   18.00  122.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       96.4842  -77.0000  150.0000 104

 19 omega   63.00  158.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       96.4842   77.0000    0.0000 95
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1075607000
_diffrn_orient_matrix_UB_12      0.0072850000
_diffrn_orient_matrix_UB_13      -0.0415366000
_diffrn_orient_matrix_UB_21      -0.0371665000
_diffrn_orient_matrix_UB_22      -0.0865679000
_diffrn_orient_matrix_UB_23      -0.0387153000
_diffrn_orient_matrix_UB_31      -0.0776583000
_diffrn_orient_matrix_UB_32      0.0514542000
_diffrn_orient_matrix_UB_33      -0.0592888000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33119
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.436
_diffrn_reflns_theta_min         3.733
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.890
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61591
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       prism
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.137
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.077
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5853
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+3.3439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5331
_reflns_number_total             5853
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501161y_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 4085329--4085336.cif.'
_cod_database_code               4085332
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         C66H64Fe2P2I2
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     63.60
_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. Rigid bond restraints
 C113, C114
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C113, C114
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
P1A \\sim C2A \\sim C2 \\sim P1 \\sim C2B \\sim P1B: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.1
4. Others
 Fixed Sof: P1(0.83122) P1A(0.10241) P1B(0.06639) C2(0.16877) H2(0.16877)
 C2A(0.8976) H2A(0.8976) C2B(0.93362) H2B(0.93362)
5.a Ternary CH refined with riding coordinates:
 C2(H2)
5.b Me refined with riding coordinates:
 C16(H16a,H16b,H16c), C17(H17a,H17b,H17c), C18(H18a,H18b,H18c), C19(H19a,H19b,
 H19c), C20(H20a,H20b,H20c)
5.c Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C2B(H2B), 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), C101(D101),
 C102(D102), C103(D103), C104(D104), C105(D105), C106(D106)
;
_shelx_res_checksum              27773
_shelx_hkl_checksum              11206
_olex2_submission_special_instructions 'No special instructions were received'