Tris(pyrazolyl)methanide Complexes of Trivalent Rare-Earth Metals
Li, Tengfei; Zhang, Guangchao; Guo, Jingjing; Wang, Shaowu; Leng, Xuebing; Chen, Yaofeng; Organometallics 35 (2016) 1565–; doi:10.1021/acs.organomet.6b00166

data_4088536
_publ_section_title
;
 Tris(pyrazolyl)methanide Complexes of Trivalent Rare-Earth Metals
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              1565
_journal_paper_doi               10.1021/acs.organomet.6b00166
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C32 H53 Cl3 Li N6 O4 Y'
_chemical_formula_weight         788.00
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   12.554(3)
_cell_length_b                   12.554(3)
_cell_length_c                   43.637(11)
_cell_measurement_reflns_used    1708
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      19.35
_cell_measurement_theta_min      2.64
_cell_volume                     5956(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0915
_diffrn_reflns_av_sigmaI/netI    0.0947
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            15020
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.60
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    1.711
_exptl_absorpt_correction_T_max  0.7482
_exptl_absorpt_correction_T_min  0.6743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brick-red
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.003(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         3030
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0587
_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^)+(0.0856P)^2^+2.6323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1628
_reflns_number_gt                2093
_reflns_number_total             3030
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00166_si_002.cif
_cod_data_source_block           mo_dm15761_0m
_cod_database_code               4088536