Alkali Metal Control over N-N Cleavage in Iron Complexes.
Grubel, Katarzyna; Brennessel, William W.; Mercado, Brandon Q.; Holland, Patrick L.; Journal of the American Chemical Society  (2014) 141120101403003–; doi:10.1021/ja507442b

data_4122959
_publ_section_title
;
 Alkali Metal Control over N-N Cleavage in Iron Complexes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              141120101403003
_journal_paper_doi               10.1021/ja507442b
_journal_year                    2014
_chemical_formula_moiety         'C74 H97 Fe3 N8 Na O2, C6 H14'
_chemical_formula_sum            'C80 H111 Fe3 N8 Na O2'
_chemical_formula_weight         1407.30
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 111.334(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9646(10)
_cell_length_b                   20.1695(17)
_cell_length_c                   16.2286(14)
_cell_measurement_reflns_used    27899
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      28.1
_cell_measurement_theta_min      3.0
_cell_volume                     3647.9(6)
_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 10
_diffrn_measured_fraction_theta_full 0.678
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID imaging plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.2316
_diffrn_reflns_av_unetI/netI     0.1580
_diffrn_reflns_Laue_measured_fraction_full 0.678
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            45259
_diffrn_reflns_point_group_measured_fraction_full 0.676
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         22.008
_diffrn_reflns_theta_min         3.316
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Unknown
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Flack x determined using 1888 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     886
_refine_ls_number_reflns         8918
_refine_ls_number_restraints     844
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1318
_refine_ls_R_factor_gt           0.0819
_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^)+(0.0763P)^2^+3.6532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1731
_refine_ls_wR_factor_ref         0.1992
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_full    0.673
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                5704
_reflns_number_total             8918
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja507442b_si_002.cif
_cod_data_source_block           1-Na
_cod_database_code               4122959
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.968
_shelx_res_checksum              12115
_shelx_hkl_checksum              52640