Alkali Metal Variation and Twisting of the FeNNFe Core in Bridging Diiron Dinitrogen Complexes.
McWilliams, Sean F.; Rodgers, Kenton R.; Lukat-Rodgers, Gudrun; Mercado, Brandon Q.; Grubel, Katarzyna; Holland, Patrick L.; Inorganic chemistry 55 (2016) 2960–2968; doi:10.1021/acs.inorgchem.5b02841

data_4347174
_publ_contact_author
;
 Prof. Patrick L. Holland        
;
_publ_section_title
;
 Alkali Metal Variation and Twisting of the FeNNFe Core in Bridging Diiron
 Dinitrogen Complexes.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2960
_journal_page_last               2968
_journal_paper_doi               10.1021/acs.inorgchem.5b02841
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C58 H82 Fe2 N6 Na2'
_chemical_formula_sum            'C58 H82 Fe2 N6 Na2'
_chemical_formula_weight         1020.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                87.308(6)
_cell_angle_beta                 88.635(6)
_cell_angle_gamma                86.240(6)
_cell_formula_units_Z            2
_cell_length_a                   11.5403(2)
_cell_length_b                   13.3443(2)
_cell_length_c                   18.4371(13)
_cell_measurement_reflns_used    25203
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.1
_cell_measurement_theta_min      2.4
_cell_volume                     2829.4(2)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_molecular_graphics
;
Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; Puschmann, H., 
OLEX2: A complete structure solution, refinement and analysis program
(2009). J. Appl. Cryst., 42, 339-341.
;
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 22.2
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0912
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            84013
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.179
_diffrn_reflns_theta_min         2.400
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    4.565
_exptl_absorpt_correction_T_max  0.712
_exptl_absorpt_correction_T_min  0.569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         10078
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0627P)^2^+4.1108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.1603
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8560
_reflns_number_total             10078
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02841_si_001.cif
_cod_data_source_block           2-Na
_cod_database_code               4347174
_shelx_estimated_absorpt_t_min   0.548
_shelx_estimated_absorpt_t_max   0.712
_shelxl_version_number           2013-4
_shelx_res_checksum              93667
_shelx_hkl_checksum              12031