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_4104817
_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            'C86 H132 Dy2 N2 O8'
_chemical_formula_weight         1646.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 105.2250(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.5427(5)
_cell_length_b                   12.0654(4)
_cell_length_c                   24.6783(8)
_cell_measurement_temperature    178(2)
_cell_volume                     4465.5(3)
_computing_cell_refinement       'Bruker SMART/SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      178(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0526
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            47317
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 'initial 50 frames recollected'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    1.710
_exptl_absorpt_correction_T_max  0.8083
_exptl_absorpt_correction_T_min  0.6945
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.170
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       0.0015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         10911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.179
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+17.9855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.1664
_reflns_number_gt                7860
_reflns_number_total             10911
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9036753_si_002.cif
_cod_data_source_block           gz23
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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_database_code               4104817