C-C Bond Formation and Related Reactions at the CNC Backbone in (smif)FeX (smif = 1,3-Di-(2-pyridyl)-2-azaallyl): Dimerizations, 3 + 2 Cyclization, and Nucleophilic Attack; Transfer Hydrogenations and Alkyne Trimerization (X = N(TMS)2, dpma = (Di-(2-pyridyl-methyl)-amide))
Brenda A. Frazier; Valerie A. Williams; Peter T. Wolczanski; Suzanne C. Bart; Karsten Meyer; Thomas R. Cundari; Emil B. Lobkovsky; Inorganic Chemistry 52 (2013) 3295–3312; doi:10.1021/ic302783y

data_4334227
_publ_section_title
;
 C-C Bond Formation and Related Reactions at the CNC Backbone in (smif)FeX
 (smif = 1,3-Di-(2-pyridyl)-2-azaallyl): Dimerizations, 3 + 2 Cyclization,
 and Nucleophilic Attack; Transfer Hydrogenations and Alkyne Trimerization
 (X = N(TMS)2, dpma = (Di-(2-pyridyl-methyl)-amide))
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3295
_journal_page_last               3312
_journal_paper_doi               10.1021/ic302783y
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C68 H84 Fe2 N8 Si4'
_chemical_formula_sum            'C68 H84 Fe2 N8 Si4'
_chemical_formula_weight         1237.49
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.361(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8897(7)
_cell_length_b                   35.0779(17)
_cell_length_c                   15.5291(8)
_cell_measurement_reflns_used    9856
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.93
_cell_measurement_theta_min      2.62
_cell_volume                     7566.0(7)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT+'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0557
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            69998
_diffrn_reflns_theta_full        26.47
_diffrn_reflns_theta_max         26.47
_diffrn_reflns_theta_min         1.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.487
_exptl_absorpt_correction_T_max  0.9761
_exptl_absorpt_correction_T_min  0.7588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_description       plate
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         15480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.634
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0606P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1141
_reflns_number_gt                10139
_reflns_number_total             15480
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302783y_si_001_3.cif
_cod_data_source_block           bf22
_cod_database_code               4334227