An Iron(II) Ylide Complex as A Masked Open-Shell Iron Alkylidene Species in Its Alkylidene-Transfer Reactions with Alkenes.
Liu, Jian; Hu, Lianrui; Wang, Lei; Chen, Hui; Deng, Liang; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b00484

data_4125557
_publ_section_title
;
 An Iron(II) Ylide Complex as A Masked Open-Shell Iron Alkylidene Species
 in Its Alkylidene-Transfer Reactions with Alkenes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b00484
_journal_year                    2017
_chemical_formula_moiety         'C49 H41 F4 Fe N2 O P, C6 H6'
_chemical_formula_sum            'C55 H47 F4 Fe N2 O P'
_chemical_formula_weight         914.76
_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             2015-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.733(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3415(11)
_cell_length_b                   21.375(3)
_cell_length_c                   21.794(3)
_cell_measurement_reflns_used    2932
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      21.33
_cell_measurement_theta_min      2.36
_cell_volume                     4351.4(10)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            31403
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.869
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0666 before and 0.0560 after correction.
The Ratio of minimum to maximum transmission is 0.9077.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.053
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         8543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1167
_refine_ls_R_factor_gt           0.0742
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1001P)^2^+12.5005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1876
_refine_ls_wR_factor_ref         0.2232
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5617
_reflns_number_total             8543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b00484_si_002.cif
_cod_data_source_block           2
_cod_original_cell_volume        4351.3(9)
_cod_database_code               4125557
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.878
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24),
  C28(H28), C29(H29), C30(H30), C33(H33), C34(H34), C36(H36), C37(H37),
 C40(H40), C41(H41), C43(H43), C44(H44), C50(H50), C51(H51), C52(H52), C53(H53),
  C54(H54), C55(H55)
2.c Fitted hexagon refined as free rotating group:
 C50(C51,C52,C53,C54,C55)
2.d Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              63517
_shelx_hkl_checksum              23879
_olex2_submission_special_instructions 'No special instructions were received'