Synthesis of Cationic N-Heterocyclic Carbene Lanthanide Bromide and the Influence of N-Heterocyclic Carbene and Lanthanide Metals
Yao, Haisheng; Zhang, Jinguo; Zhang, Yong; Sun, Hongmei; Shen, Qi; Organometallics 29 (2010) 5841–; doi:10.1021/om100562q

data_4066656
_publ_section_title
;
 Synthesis of Cationic N-Heterocyclic Carbene Lanthanide Bromide and the
 Influence of N-Heterocyclic Carbene and Lanthanide Metals
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5841
_journal_paper_doi               10.1021/om100562q
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C54 H88 Li2 N6 O2, 2(C4 H8 O)'
_chemical_formula_sum            'C62 H104 Li2 N6 O4'
_chemical_formula_weight         1011.39
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.244(5)
_cell_angle_beta                 106.510(9)
_cell_angle_gamma                99.210(4)
_cell_formula_units_Z            1
_cell_length_a                   10.132(6)
_cell_length_b                   11.482(6)
_cell_length_c                   14.418(8)
_cell_measurement_reflns_used    4560
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     1527.5(15)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_sigmaI/netI    0.1013
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10748
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5302
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.1568
_refine_ls_R_factor_gt           0.1066
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1115P)^2^+0.4550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2501
_refine_ls_wR_factor_ref         0.2850
_reflns_number_gt                3476
_reflns_number_total             5302
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100562q_si_001.cif
_cod_data_source_block           complex1
_cod_original_cell_volume        1527.6(14)
_cod_database_code               4066656