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_4088540
_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_moiety         'C47 H42 Lu2 N16 Si'
_chemical_formula_sum            'C46 H66 Lu2 N16 Si'
_chemical_formula_weight         1220.17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           59
_space_group_name_Hall           '-P 2ab 2a'
_space_group_name_H-M_alt        'P m m n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-11-05
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8939(13)
_cell_length_b                   17.3468(17)
_cell_length_c                   11.7131(11)
_cell_measurement_reflns_used    9328
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.29
_cell_measurement_theta_min      2.27
_cell_volume                     2823.0(5)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_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_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28626
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.581
_diffrn_reflns_theta_min         1.878
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.542
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1217 before and 0.0488 after correction.
The Ratio of minimum to maximum transmission is 0.6765.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       block
_exptl_crystal_F_000             1218
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.058
_refine_diff_density_min         -3.135
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         4619
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0557P)^2^+13.6609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1185
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3832
_reflns_number_total             4619
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00166_si_002.cif
_cod_data_source_block           dm15658
_cod_original_sg_symbol_H-M      'P m m n'
_cod_database_code               4088540
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.568
_shelx_estimated_absorpt_t_min   0.510
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C1 \\sim N4 \\sim N2: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C1) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(N5) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N1) \\sim
Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5)
\\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(N4) \\sim Ueq, Uanis(N3) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
3. Others
 Fixed Sof: C8(0.5) C7(0.5) C9(0.5) C16(0.5) C15(0.25) H15(0.25) C12(0.25)
 H12(0.25) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C17(0.5) H17A(0.5) H17B(0.5)
 H17C(0.5) C13(0.5) Si1(0.25) C10(0.5) C11(0.5) C20(0.5) C19(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C15(H15), C12(H12)
4.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C2(H2A,H2B,H2C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              69394
_shelx_hkl_checksum              17373
_olex2_submission_special_instructions 'No special instructions were received'