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_4334228
_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_sum            'C54 H62 Fe N8 O3'
_chemical_formula_weight         926.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           54
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2ac'
_symmetry_space_group_name_H-M   'P c c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.168(5)
_cell_length_b                   17.174(3)
_cell_length_c                   18.038(3)
_cell_measurement_reflns_used    2049
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      16.13
_cell_measurement_theta_min      2.34
_cell_volume                     10585(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1560
_diffrn_reflns_av_sigmaI/netI    0.1149
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            57325
_diffrn_reflns_theta_full        20.87
_diffrn_reflns_theta_max         20.87
_diffrn_reflns_theta_min         1.68
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.333
_exptl_absorpt_correction_T_max  0.9901
_exptl_absorpt_correction_T_min  0.8647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       needle
_exptl_crystal_F_000             3936
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_platon_squeeze_details          ' '
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.00050(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         5564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.1284
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0911P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1702
_reflns_number_gt                2984
_reflns_number_total             5564
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302783y_si_001_4.cif
_cod_data_source_block           m
_cod_database_code               4334228