Synthesis and Catalytic Property of Iron Pincer Complexes Generated by Csp3‒H Activation
Zhao, Hua; Sun, Hongjian; Li, Xiaoyan; Organometallics  (2014) 140701152748009–; doi:10.1021/om500429r

data_4083857
_publ_section_title
;
 Synthesis and Catalytic Property of Iron Pincer Complexes Generated by
 Csp3--H Activation
;
_journal_name_full               Organometallics
_journal_page_first              140701152748009
_journal_paper_doi               10.1021/om500429r
_journal_year                    2014
_chemical_formula_moiety         'C43 H48 Fe P4'
_chemical_formula_sum            'C43 H48 Fe P4'
_chemical_formula_weight         744.54
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-05-09
_audit_creation_method
; 
  Olex2 1.2 
  (compiled Apr  9 2013 14:06:00, GUI svn.r4458) 
;
_cell_angle_alpha                108.38(3)
_cell_angle_beta                 104.18(3)
_cell_angle_gamma                97.70(3)
_cell_formula_units_Z            4
_cell_length_a                   10.741(2)
_cell_length_b                   18.843(4)
_cell_length_c                   21.735(4)
_cell_measurement_temperature    293(2)
_cell_volume                     3939.3(18)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics
; 
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, 
OLEX2: a complete structure solution, refinement and analysis program. 
J. Appl. Cryst. (2009). 42, 339-341. 
;
_computing_publication_material
; 
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, 
OLEX2: a complete structure solution, refinement and analysis program. 
J. Appl. Cryst. (2009). 42, 339-341. 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0929
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            23197
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.04
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_T_max  0.8938
_exptl_absorpt_correction_T_min  0.8745
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.742
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     893
_refine_ls_number_reflns         16918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.742
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.055
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1344P)^2^+7.1809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1460
_refine_ls_wR_factor_ref         0.1954
_reflns_number_gt                10536
_reflns_number_total             16918
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500429r_si_001.cif
_cod_data_source_block           complex2
_cod_original_cell_volume        3939.3(14)
_cod_database_code               4083857
_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 Aromatic/amide H refined with riding coordinates: 
 C86(H86), C85(H85), C2(H2A), C3(H3), C37(H37), C22(H22), C6(H6), C8(H8), 
 C13(H13), C25(H25), C4(H4), C16(H16), C35(H35), C10(H10), C12(H12), C36(H36), 
 C5(H5), C17(H17), C24(H24), C29(H29), C28(H28), C23(H23), C27(H27), C9(H9), 
 C31(H31), C34(H34), C18(H18), C30(H30), C33(H33), C11(H11), C58(H58), C62(H62), 
  C61(H61), C59(H59), C57(H57), C47(H47), C44(H44), C67(H67), C66(H66), 
 C69(H69), C64(H64), C65(H65), C71(H71), C63(H63), C68(H68), C76(H76), C75(H75), 
  C70(H70), C77(H77), C74(H74), C73(H73), C72(H72), C78(H78), C84(H84), 
 C83(H83), C82(H82) 
2.b Idealised Me refined as rotating group: 
 C40(H40A,H40B,H40C), C43(H43A,H43B,H43C), C41(H41A,H41B,H41C), C38(H38A,H38B, 
 H38C), C42(H42A,H42B,H42C), C39(H39A,H39B,H39C), C54(H54A,H54B,H54C), C53(H53A, 
 H53B,H53C), C55(H55A,H55B,H55C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), 
 C79(H79A,H79B,H79C) 
;