Electronic Structure Determination of Pyridine N-Heterocyclic Carbene Iron Dinitrogen Complexes and Neutral Ligand Derivatives.
Darmon, Jonathan M.; Yu, Renyuan Pony; Semproni, Scott P.; Turner, Zoë R; Stieber, S Chantal E; DeBeer, Serena; Chirik, Paul J.; Organometallics 33 (2014) 5423–5433; doi:10.1021/om500727t

data_4084376
_publ_section_title
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 Electronic Structure Determination of Pyridine N-Heterocyclic Carbene
 Iron Dinitrogen Complexes and Neutral Ligand Derivatives.
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5423
_journal_page_last               5433
_journal_paper_doi               10.1021/om500727t
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C46 H61 Fe N9 O'
_chemical_formula_weight         811.89
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 92.883(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   11.098(5)
_cell_length_b                   23.513(5)
_cell_length_c                   16.613(5)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.56
_cell_measurement_theta_min      4.61
_cell_volume                     4330(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, 2008)'
_computing_structure_solution    'SIR92 (Giacavazzo 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            45763
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         66.34
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    3.145
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.083
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         7424
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0314
_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^+1.7647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0858
_reflns_number_gt                6845
_reflns_number_total             7424
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om500727t_si_002.cif
_cod_data_source_block           jmd20
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4084375--4084376.cif.
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_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4084376