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_4088539
_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            'C28 H51 Lu N6 O Si2'
_chemical_formula_weight         718.89
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 105.7480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8087(8)
_cell_length_b                   14.4867(10)
_cell_length_c                   21.0202(14)
_cell_measurement_reflns_used    7189
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      28.11
_cell_measurement_theta_min      2.28
_cell_volume                     3460.9(4)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            34456
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.579
_diffrn_reflns_theta_min         1.729
_exptl_absorpt_coefficient_mu    2.950
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.348
_refine_diff_density_min         -1.053
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         10616
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+0.8999P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7976
_reflns_number_total             10616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00166_si_002.cif
_cod_data_source_block           mo_dm15102_0m
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4088539
_shelx_estimated_absorpt_t_min   0.590
_shelx_estimated_absorpt_t_max   0.798
_shelxl_version_number           2014-3
_shelx_res_checksum              60665
_shelx_hkl_checksum              16871