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_4088537
_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_absolute_configuration ad
_chemical_formula_sum            'C32 H53 Cl3 Li Lu N6 O4'
_chemical_formula_weight         874.06
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   12.5731(12)
_cell_length_b                   12.5731(12)
_cell_length_c                   43.468(4)
_cell_measurement_reflns_used    5388
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.17
_cell_measurement_theta_min      2.65
_cell_volume                     5950.9(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0383
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_number            18902
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.765
_diffrn_reflns_theta_min         2.092
_exptl_absorpt_coefficient_mu    2.731
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brick-red
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       block
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
; 
 Flack x determined using 1423 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.008(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         4113
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+1.8107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0814
_reflns_Friedel_coverage         0.988
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                3059
_reflns_number_total             4113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00166_si_002.cif
_cod_data_source_block           mo_dm14564_0m
_cod_original_cell_volume        5950.9(13)
_cod_database_code               4088537
_shelx_estimated_absorpt_t_min   0.548
_shelx_estimated_absorpt_t_max   0.735
_shelxl_version_number           2014-3
_shelx_res_checksum              58650
_shelx_hkl_checksum              11013