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_4085330
_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         'C45 H58 Fe K O7 P, 1.5(C4 H8 O)'
_chemical_formula_sum            'C51 H70 Fe K O8.5 P'
_chemical_formula_weight         944.99
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-08-28
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 125.939(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.9659(6)
_cell_length_b                   20.6879(4)
_cell_length_c                   22.0458(4)
_cell_measurement_reflns_used    20995
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      28.7280
_cell_measurement_theta_min      3.3970
_cell_volume                     9957.5(4)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49)'
_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 7.9851
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   -8.00   84.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8664   77.0000  -60.0000 184

  2 omega   -4.00   61.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8664   57.0000   30.0000 130

  3 omega  -40.00   51.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2571   57.0000 -150.0000 182

  4 omega  -87.00    3.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.2571  -57.0000   60.0000 180

  5 omega   35.00   94.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8664  178.0000 -150.0000 118

  6 omega  -12.00   13.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8664   77.0000 -180.0000 50

  7 omega  -55.00   43.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8664  -38.0000  -30.0000 196
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0009357500
_diffrn_orient_matrix_UB_12      0.0019364500
_diffrn_orient_matrix_UB_13      -0.0318378500
_diffrn_orient_matrix_UB_21      0.0100415000
_diffrn_orient_matrix_UB_22      0.0325585000
_diffrn_orient_matrix_UB_23      0.0048596000
_diffrn_orient_matrix_UB_31      0.0308698500
_diffrn_orient_matrix_UB_32      -0.0106360500
_diffrn_orient_matrix_UB_33      0.0089965500
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            49205
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.967
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_description       block
_exptl_crystal_F_000             4032
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         9767
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+26.4571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1185
_refine_ls_wR_factor_ref         0.1226
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8495
_reflns_number_total             9767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501161y_si_002.cif
_cod_data_source_block           K2
_cod_depositor_comments
'Adding full bibliography for 4085329--4085336.cif.'
_cod_original_formula_sum        'C51 H70 Fe K O8.50 P'
_cod_database_code               4085330
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C45 H57 Fe K O6 P'
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H40A,H40B} of C40, {H39A,H39B} of C39, {H42A,H42B} of C42,
   {H36A,H36B} of C36, {H38A,H38B} of C38, {H41A,H41B} of C41, {H35A,H35B} of
  C35, {H34A,H34B} of C34, {H45A,H45B} of C45, {H44A,H44B} of C44, {H43A,H43B}
  of C43, {H37A,H37B} of C37, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H50E,H50F} of C503, {H50C,H50D} of C502, {H50A,H50B}
  of C501, {H50G,H50H} of C504, {H20G,H20H} of C203, {H20E,H20F} of C202
2. Restrained distances
 O9A-C201 \\sim O9-C201 \\sim O9A-C204 \\sim O9-C204
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O10 \\sim C504 \\sim C503 \\sim C502 \\sim C501: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02
O9A \\sim O9: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O9(0.75) O9A(0.25) H20A(0.75) H20B(0.75) H20C(0.25) H20D(0.25)
 H20I(0.75) H20J(0.75) H20K(0.25) H20L(0.25) O10(0.5) C501(0.5) H50A(0.5)
 H50B(0.5) C502(0.5) H50C(0.5) H50D(0.5) C503(0.5) H50E(0.5) H50F(0.5)
 C504(0.5) H50G(0.5) H50H(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,
 H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B),
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C201(H20A,H20B), C201(H20C,
 H20D), C202(H20E,H20F), C203(H20G,H20H), C204(H20I,H20J), C204(H20K,H20L),
 C501(H50A,H50B), C502(H50C,H50D), C503(H50E,H50F), C504(H50G,H50H)
5.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24),
 C25(H25), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33)
5.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              7273
_shelx_hkl_checksum              27863
_olex2_submission_special_instructions 'No special instructions were received'