Synthesis and structural characterization of imido‒lanthanide complexes with a metal‒nitrogen multiple bond
Chan, Hoi-Shan; Li, Hung-Wing; Xie, Zuowei; Chemical Communications  (2002) 652–; doi:10.1039/b110793c

data_7114321
_publ_section_title
;
 Synthesis and structural characterization of imido--lanthanide complexes
 with a metal--nitrogen multiple bond
;
_journal_issue                   6
_journal_name_full               'Chemical Communications'
_journal_page_first              652
_journal_paper_doi               10.1039/b110793c
_journal_year                    2002
_chemical_formula_sum            'C52 H80 N4 Na O Yb'
_chemical_formula_weight         973.23
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 117.6830(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.5164(11)
_cell_length_b                   19.8148(10)
_cell_length_c                   24.5415(12)
_cell_measurement_temperature    293(2)
_cell_volume                     10557.3(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0860
_diffrn_reflns_av_sigmaI/netI    0.1324
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            58633
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    1.817
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7206
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4072
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.000042(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.809
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1067
_refine_ls_number_reflns         18578
_refine_ls_number_restraints     189
_refine_ls_restrained_S_all      0.817
_refine_ls_R_factor_all          0.1206
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.00
_refine_ls_shift/su_mean         0.00
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0927
_reflns_number_gt                8502
_reflns_number_total             18578
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b110793c.txt
_cod_data_source_block           complex_1
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7114321