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_4347176
_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 Cs2 Fe2 N6'
_chemical_formula_sum            'C58 H82 Cs2 Fe2 N6'
_chemical_formula_weight         1240.81
_space_group_crystal_system      tetragonal
_space_group_IT_number           81
_space_group_name_Hall           'P -4'
_space_group_name_H-M_alt        'P -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.4609(3)
_cell_length_b                   16.4609(3)
_cell_length_c                   10.6149(8)
_cell_measurement_reflns_used    59368
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      66.7
_cell_measurement_theta_min      6.8
_cell_volume                     2876.2(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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 22.2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1734
_diffrn_reflns_av_unetI/netI     0.0728
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            86104
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.532
_diffrn_reflns_theta_max         66.532
_diffrn_reflns_theta_min         6.807
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    14.067
_exptl_absorpt_correction_T_max  0.766
_exptl_absorpt_correction_T_min  0.544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.304
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.188
_refine_ls_abs_structure_details
; 
 Flack x determined using 1622 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.003(6)
_refine_ls_extinction_coef       0.0056(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         5078
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0658
_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^)+(0.1152P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1646
_refine_ls_wR_factor_ref         0.1798
_reflns_Friedel_coverage         0.886
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4246
_reflns_number_total             5078
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02841_si_001.cif
_cod_data_source_block           2-Cs
_cod_database_code               4347176
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.243
_shelx_estimated_absorpt_t_max   0.766
_shelx_res_checksum              39950
_shelx_hkl_checksum              1461