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_4122960
_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         'C88 H108 Cl2 Fe4 N10 Rb2, C6 H14'
_chemical_formula_sum            'C94 H122 Cl2 Fe4 N10 Rb2'
_chemical_formula_weight         1857.26
_chemical_name_common            holkg19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.857(2)
_cell_angle_beta                 104.953(2)
_cell_angle_gamma                109.636(2)
_cell_formula_units_Z            2
_cell_length_a                   14.8536(16)
_cell_length_b                   18.951(2)
_cell_length_c                   19.309(2)
_cell_measurement_reflns_used    3972
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      29.48
_cell_measurement_theta_min      2.35
_cell_volume                     4794.5(9)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_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  0.0751
_diffrn_reflns_av_sigmaI/netI    0.0814
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            110243
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.54
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.705
_exptl_absorpt_correction_T_max  0.8216
_exptl_absorpt_correction_T_min  0.5635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.258
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1093
_refine_ls_number_reflns         29201
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1216
_reflns_number_gt                18548
_reflns_number_total             29201
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja507442b_si_002.cif
_cod_data_source_block           1-Rb
_cod_original_cell_volume        4794.6(9)
_cod_database_code               4122960