Rare-earth metal-mediated PhC[triple bond, length as m-dash]N insertion into N,N-bis(trimethylsilyl)naphthalene-1,8-diamido dianion - a synthetic approach to complexes coordinated by ansa-bridged amido-amidinato ligand.
Lyubov, Dmitry M.; Cherkasov, Anton V.; Fukin, Georgy K.; Lyssenko, Konstantin A.; Rychagova, Elena A.; Ketkov, Sergey Yu; Trifonov, Alexander A.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 438–451; doi:10.1039/c7dt03809g

data_7044763
_publ_section_title
;
 Rare-earth metal-mediated PhC[triple bond, length as m-dash]N insertion
 into N,N-bis(trimethylsilyl)naphthalene-1,8-diamido dianion - a synthetic
 approach to complexes coordinated by ansa-bridged amido-amidinato ligand.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              438
_journal_page_last               451
_journal_paper_doi               10.1039/c7dt03809g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C46 H59 Cl N6 Si4 Sm, C12 H30 Li O6, C4 H10 O2'
_chemical_formula_sum            'C62 H99 Cl Li N6 O8 Si4 Sm'
_chemical_formula_weight         1361.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2017-11-07 deposited with the CCDC.
2017-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.3740(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4061(4)
_cell_length_b                   27.5182(9)
_cell_length_c                   20.9997(7)
_cell_measurement_reflns_used    5932
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.22
_cell_volume                     7137.7(4)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXL-2017/1
_computing_structure_solution    SHELXT-2014/5
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex (CCD)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            56772
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.039
_diffrn_reflns_theta_max         25.039
_diffrn_reflns_theta_min         1.948
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.979
_exptl_absorpt_correction_T_max  0.837
_exptl_absorpt_correction_T_min  0.673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS 2016/2: L. Krause et al., J. Appl. Cryst., 2015, 48, 3-10
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       stick
_exptl_crystal_F_000             2860
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.812
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     868
_refine_ls_number_reflns         12602
_refine_ls_number_restraints     612
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1050P)^2^+16.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1798
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9540
_reflns_number_total             12602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03809g2.cif
_cod_data_source_block           3SM
_cod_depositor_comments
'Adding full bibliography for 7044761--7044767.cif.'
_cod_original_cell_volume        7137.6(4)
_cod_database_code               7044763
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.662
_shelx_estimated_absorpt_t_max   0.900
_shelx_res_checksum              37840