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_4134939
_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            'C76 H190 Gd2 K2 N8 O19 Si12'
_chemical_formula_weight         2250.13
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                78.975(2)
_cell_angle_beta                 77.363(2)
_cell_angle_gamma                82.456(3)
_cell_formula_units_Z            2
_cell_length_a                   15.658(3)
_cell_length_b                   16.014(3)
_cell_length_c                   24.347(4)
_cell_measurement_reflns_used    9456
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.93
_cell_measurement_theta_min      2.34
_cell_volume                     5821.6(18)
_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 0.913
_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  0.0435
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            72119
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.096
_diffrn_reflns_theta_min         1.438
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.381
_exptl_absorpt_correction_T_max  0.4318
_exptl_absorpt_correction_T_min  0.3904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.374
_exptl_crystal_size_mid          0.259
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.588
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1123
_refine_ls_number_reflns         28562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+6.4292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1129
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20565
_reflns_number_total             28562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01021_si_003.cif
_cod_data_source_block           ajr33
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not_measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
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_cod_original_cell_volume        5821.7(18)
_cod_database_code               4134939
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.626
_shelx_estimated_absorpt_t_max   0.770
_exptl_absorpt_special_details
; 
Reflections not merged 
72119 Corrected reflections written to file ajr33s.hkl 
Estimated minimum and maximum transmission:  0.3904  0.4318 
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              96089
_shelx_hkl_checksum              60315