Formation of the End-on Bound Lanthanide Dinitrogen Complexes, [(R2N)3Ln-N=N-Ln(NR2)3]2-, from Divalent [(R2N)3Ln]1- Salts (R = SiMe3).
Ryan, Austin J.; Balasubramani, Sreeganesh; Ziller, Joseph W.; Furche, Filipp; Evans, William J.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c01021

data_4134940
_publ_section_title
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 Formation of the End-on Bound Lanthanide Dinitrogen Complexes,
 [(R2N)3Ln-N=N-Ln(NR2)3]2-, from Divalent [(R2N)3Ln]1- Salts (R = SiMe3).
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_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c01021
_journal_year                    2020
_chemical_formula_sum            'C80 H200 K2 N12 O14 Si12 Tb2'
_chemical_formula_weight         2287.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                102.9109(17)
_cell_angle_beta                 96.0143(17)
_cell_angle_gamma                104.6636(17)
_cell_formula_units_Z            2
_cell_length_a                   15.437(2)
_cell_length_b                   16.218(2)
_cell_length_c                   26.133(3)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.83
_cell_measurement_theta_min      2.35
_cell_volume                     6078.5(13)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            75362
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.178
_diffrn_reflns_theta_min         1.623
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.394
_exptl_absorpt_correction_T_max  0.4319
_exptl_absorpt_correction_T_min  0.3842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       square
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.143
_refine_diff_density_max         1.500
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1139
_refine_ls_number_reflns         29882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+1.8589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23503
_reflns_number_total             29882
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01021_si_002.cif
_cod_data_source_block           ajr27
_cod_original_cell_volume        6078.6(14)
_cod_database_code               4134940
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.714
_shelx_estimated_absorpt_t_max   0.826
_exptl_absorpt_special_details
; 
  
 Reflections not merged 
   75369 Corrected reflections written to file ajr27s.hkl 
 Estimated minimum and maximum transmission:  0.3842  0.4319 
 The ratio of these values is more reliable than their absolute values! 
 Additional spherical absorption correction applied with mu*r =  0.6000 
 Lambda/2 correction factor = 0.00150 
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_shelx_res_checksum              14915
_shelx_hkl_checksum              53659