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_7044767
_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         'C33 H54 N5 O Si2 Y'
_chemical_formula_sum            'C33 H54 N5 O Si2 Y'
_chemical_formula_weight         681.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.749(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4113(7)
_cell_length_b                   27.1287(14)
_cell_length_c                   12.0915(8)
_cell_measurement_reflns_used    4715
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.9370
_cell_measurement_theta_min      3.4750
_cell_volume                     3709.0(4)
_computing_cell_refinement       'CrysAlis PRO'
_computing_data_collection       'CrysAlis PRO'
_computing_data_reduction        'CrysAlis PRO'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXL-2017/1
_computing_structure_solution    SHELXT-2014/5
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur EOS (CCD)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21981
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         3.004
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    1.668
_exptl_absorpt_correction_T_max  0.729
_exptl_absorpt_correction_T_min  0.721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis PRO 1.171.38.43. Spherical absorption correction using equivalent
radius and absorption coefficient. Empirical absorption correction
using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       prism
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         9572
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+0.7400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0955
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6763
_reflns_number_total             9572
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03809g2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7044761--7044767.cif.'
_cod_database_code               7044767
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.555
_shelx_estimated_absorpt_t_max   0.788
_shelx_res_checksum              53337