Synthesis of the (N2)3- Radical from Y2+ and Its Protonolysis Reactivity To Form (N2H2)2- via the Y[N(SiMe3)2]3/KC8 Reduction System
Ming Fang; David S. Lee; Joseph W. Ziller; Robert J. Doedens; Jefferson E. Bates; Filipp Furche; William J. Evans; Journal of the American Chemical Society 133 (2011) 3784–3787; doi:10.1021/ja1116827

data_4105789
_publ_section_title
;
 Synthesis of the (N2)3- Radical from Y2+ and Its Protonolysis Reactivity
 To Form (N2H2)2- via the Y[N(SiMe3)2]3/KC8 Reduction System
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3784
_journal_page_last               3787
_journal_paper_doi               10.1021/ja1116827
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C32 H88 Gd2 N6 O2 Si8'
_chemical_formula_weight         1128.30
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.64(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.865(4)
_cell_length_b                   23.466(5)
_cell_length_c                   11.602(2)
_cell_measurement_reflns_used    6814
_cell_measurement_temperature    161(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.2
_cell_volume                     2730.1(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      161(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '25s frames at 0.3 deg omega increments'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28237
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    2.614
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'computed via SADABS (Sheldrick, Gottingen)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         6565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.025P)^2^+2.75P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0672
_reflns_number_gt                5375
_reflns_number_total             6565
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1116827_si_004.cif
_cod_data_source_block           dl18
_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_original_cell_volume        2730.1(12)
_cod_database_code               4105789