Isolation of Dysprosium and Yttrium Complexes of a Three-Electron Reduction Product in the Activation of Dinitrogen, the (N2)3- Radical
William J. Evans; Ming Fang; Gaël Zucchi; Filipp Furche; Joseph W. Ziller; Ryan M. Hoekstra; Jeffrey I. Zink; Journal of the American Chemical Society 131 (2009) 11195–11202; doi:10.1021/ja9036753

data_4104821
_publ_section_title
;
 Isolation of Dysprosium and Yttrium Complexes of a Three-Electron
 Reduction Product in the Activation of Dinitrogen, the (N2)3- Radical
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11195
_journal_page_last               11202
_journal_paper_doi               10.1021/ja9036753
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C35.5 H92 K N6 O2 Si8 Y2'
_chemical_formula_weight         1076.79
_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           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 105.071(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.481(3)
_cell_length_b                   21.371(5)
_cell_length_c                   22.304(5)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      2.34
_cell_volume                     5745(2)
_computing_cell_refinement       'Bruker SMART APEX2/SAINT'
_computing_data_collection       'Bruker SMART APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'phi and omega'
_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  0.0707
_diffrn_reflns_av_sigmaI/netI    0.0557
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            65005
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    2.282
_exptl_absorpt_correction_T_max  0.8944
_exptl_absorpt_correction_T_min  0.6457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.437
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         12646
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0364P)^2^+6.1800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0910
_reflns_number_gt                9448
_reflns_number_total             12646
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9036753_si_006.cif
_cod_data_source_block           mf8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        5744(2)
_cod_original_formula_sum        'C35.50 H92 K N6 O2 Si8 Y2'
_cod_database_code               4104821