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_4134942
_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_absolute_configuration unk
_chemical_formula_sum            'C58 H146 Gd2 K N7 O7 Si10'
_chemical_formula_weight         1688.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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                90
_cell_angle_beta                 93.7131(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.6104(11)
_cell_length_b                   20.7558(17)
_cell_length_c                   16.9683(14)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.79
_cell_measurement_theta_min      2.19
_cell_volume                     4431.9(6)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10403
_diffrn_reflns_point_group_measured_fraction_full 0.515
_diffrn_reflns_point_group_measured_fraction_max 0.514
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         1.552
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.709
_exptl_absorpt_correction_T_max  0.745829
_exptl_absorpt_correction_T_min  0.745829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS 2012/1'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          0.465
_exptl_crystal_size_mid          0.460
_exptl_crystal_size_min          0.440
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details
; 
No quotients, so Flack parameter determined by classical intensity fit 
;
_refine_ls_abs_structure_Flack   0.115(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         10403
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0462P)^2^+8.2544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0862
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                10154
_reflns_number_total             10403
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01021_si_005.cif
_cod_data_source_block           ajr56
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4134942
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.504
_shelx_estimated_absorpt_t_max   0.520
_exptl_absorpt_special_details
; 
HKLF 5 dataset constructed from all observations involving domain 1 
   19238 Corrected reflections written to file twin5.hkl 
 Reflections merged according to point-group 2/m 
 Single reflections that also occur in composites omitted 
 Minimum and maximum apparent transmission:  0.617083  0.745829 
 Additional spherical absorption correction applied with mu*r =  0.2000 
;
_shelx_res_checksum              69512
_shelx_hkl_checksum              81459