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_4334225
_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         'C40 H64 Fe2 N8 Si4'
_chemical_formula_sum            'C40 H64 Fe2 N8 Si4'
_chemical_formula_weight         881.05
_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                 104.629(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.1297(5)
_cell_length_b                   18.5891(9)
_cell_length_c                   14.2734(9)
_cell_measurement_reflns_used    7615
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.01
_cell_measurement_theta_min      2.19
_cell_volume                     2343.9(2)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22647
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.19
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  0.8949
_exptl_absorpt_correction_T_min  0.7515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.978
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5817
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0491P)^2^+0.8812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0991
_reflns_number_gt                4615
_reflns_number_total             5817
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302783y_si_001_1.cif
_cod_data_source_block           vw16
_cod_original_cell_volume        2343.8(2)
_cod_database_code               4334225