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_4134943
_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            'C84 H210 Gd2 K2 N12 O15 Si12'
_chemical_formula_weight         2358.41
_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     'dual space'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                75.118(3)
_cell_angle_beta                 79.221(3)
_cell_angle_gamma                76.734(3)
_cell_formula_units_Z            2
_cell_length_a                   15.237(3)
_cell_length_b                   20.708(5)
_cell_length_c                   21.341(5)
_cell_measurement_reflns_used    9041
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28.61
_cell_measurement_theta_min      2.44
_cell_volume                     6275(2)
_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      133(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.902
_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  0.0266
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.902
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            74933
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.894
_diffrn_reflns_theta_min         1.267
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.283
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.388
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.145
_refine_diff_density_max         2.899
_refine_diff_density_min         -1.426
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1202
_refine_ls_number_reflns         29795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0358P)^2^+6.1733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23770
_reflns_number_total             29795
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01021_si_004.cif
_cod_data_source_block           ajr50
_cod_database_code               4134943
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.636
_shelx_estimated_absorpt_t_max   0.836
_exptl_absorpt_special_details
; 
  
 Reflections not merged 
   74935 Corrected reflections written to file ajr50s.hkl 
 Estimated minimum and maximum transmission:  0.6575  0.7458 
 The ratio of these values is more reliable than their absolute values! 
 Additional spherical absorption correction applied with mu*r =  0.2000 
 Lambda/2 correction factor = 0.00150 
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_shelx_res_checksum              58649
_shelx_hkl_checksum              4444