#------------------------------------------------------------------------------
#$Date: 2025-08-21 14:03:24 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301848 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/24/7022400.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7022400
loop_
_publ_author_name
'Li, Qinghai'
'Zhou, Shuangliu'
'Wang, Shaowu'
'Zhu, Xiancui'
'Zhang, Lijun'
'Feng, Zhijun'
'Guo, Liping'
'Wang, Fenhua'
'Wei, Yun'
_publ_section_title
;
 Dehydrogenation of secondary amines: synthesis, and characterization of
 rare-earth metal complexes incorporating imino- or amido-functionalized
 pyrrolyl ligands.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2861
_journal_page_last               2869
_journal_paper_doi               10.1039/c2dt32513f
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C46 H80 N6 Nd2 Si4'
_chemical_formula_weight         1118.00
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 103.536(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.619(5)
_cell_length_b                   12.344(3)
_cell_length_c                   17.358(4)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.29
_cell_volume                     5545(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_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  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19673
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    1.972
_exptl_absorpt_correction_T_max  0.7304
_exptl_absorpt_correction_T_min  0.6598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            bluish
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.763
_refine_diff_density_min         -0.986
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5423
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0396
_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/[σ²(Fo²)+(0.0359P)²+34.4879P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.1167
_reflns_number_gt                4127
_reflns_number_total             5423
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32513f.txt
_cod_data_source_block           7a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7022400
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C -0.0340(2) 0.4629(6) 0.1204(3) 0.0565(16) Uani 1 1 d .
H1 H -0.0241 0.3942 0.1404 0.068 Uiso 1 1 calc R
C2 C -0.0814(3) 0.5094(7) 0.1167(4) 0.070(2) Uani 1 1 d .
H2 H -0.1090 0.4780 0.1328 0.084 Uiso 1 1 calc R
C3 C -0.0803(2) 0.6128(6) 0.0842(4) 0.0633(18) Uani 1 1 d .
H3 H -0.1070 0.6632 0.0737 0.076 Uiso 1 1 calc R
C4 C -0.0314(2) 0.6251(5) 0.0707(4) 0.0502(14) Uani 1 1 d .
C5 C -0.0069(2) 0.7263(5) 0.0481(5) 0.0627(17) Uani 1 1 d .
H5A H -0.0262 0.7505 -0.0035 0.075 Uiso 1 1 calc R
H5B H -0.0087 0.7829 0.0862 0.075 Uiso 1 1 calc R
C6 C 0.0756(2) 0.8081(4) 0.0552(3) 0.0439(12) Uani 1 1 d .
C7 C 0.0761(2) 0.8746(5) -0.0102(4) 0.0531(14) Uani 1 1 d .
C8 C 0.1078(3) 0.9647(6) 0.0001(5) 0.077(2) Uani 1 1 d .
H8 H 0.1089 1.0080 -0.0433 0.092 Uiso 1 1 calc R
C9 C 0.1372(4) 0.9911(7) 0.0727(6) 0.089(3) Uani 1 1 d .
H9 H 0.1588 1.0514 0.0784 0.107 Uiso 1 1 calc R
C10 C 0.1354(3) 0.9301(6) 0.1370(5) 0.078(2) Uani 1 1 d .
H10 H 0.1550 0.9504 0.1866 0.093 Uiso 1 1 calc R
C11 C 0.1046(2) 0.8377(5) 0.1302(4) 0.0543(15) Uani 1 1 d .
C12 C 0.0430(3) 0.8494(6) -0.0914(4) 0.0656(18) Uani 1 1 d .
H12 H 0.0244 0.7819 -0.0871 0.079 Uiso 1 1 calc R
C13 C 0.0023(4) 0.9378(7) -0.1199(5) 0.093(3) Uani 1 1 d .
H13A H 0.0193 1.0052 -0.1246 0.140 Uiso 1 1 calc R
H13B H -0.0188 0.9455 -0.0823 0.140 Uiso 1 1 calc R
H13C H -0.0190 0.9178 -0.1705 0.140 Uiso 1 1 calc R
C14 C 0.0747(4) 0.8313(8) -0.1527(5) 0.096(3) Uani 1 1 d .
H14A H 0.0998 0.7754 -0.1345 0.145 Uiso 1 1 calc R
H14B H 0.0921 0.8972 -0.1601 0.145 Uiso 1 1 calc R
H14C H 0.0523 0.8097 -0.2020 0.145 Uiso 1 1 calc R
C15 C 0.1023(3) 0.7739(6) 0.2046(4) 0.0672(18) Uani 1 1 d .
H15 H 0.0806 0.7100 0.1882 0.081 Uiso 1 1 calc R
C16 C 0.0775(5) 0.8409(11) 0.2588(6) 0.144(5) Uani 1 1 d .
H16A H 0.1005 0.8982 0.2818 0.216 Uiso 1 1 calc R
H16B H 0.0706 0.7956 0.3000 0.216 Uiso 1 1 calc R
H16C H 0.0457 0.8712 0.2287 0.216 Uiso 1 1 calc R
C17 C 0.1539(4) 0.7357(9) 0.2510(6) 0.114(3) Uani 1 1 d .
H17A H 0.1726 0.7956 0.2793 0.171 Uiso 1 1 calc R
H17B H 0.1731 0.7060 0.2154 0.171 Uiso 1 1 calc R
H17C H 0.1492 0.6810 0.2880 0.171 Uiso 1 1 calc R
C18 C 0.2008(4) 0.4262(8) 0.2706(4) 0.091(3) Uani 1 1 d .
H18A H 0.1881 0.4936 0.2860 0.137 Uiso 1 1 calc R
H18B H 0.2371 0.4325 0.2732 0.137 Uiso 1 1 calc R
H18C H 0.1951 0.3698 0.3057 0.137 Uiso 1 1 calc R
C19 C 0.1954(4) 0.2690(7) 0.1379(6) 0.109(3) Uani 1 1 d .
H19A H 0.2302 0.2840 0.1347 0.163 Uiso 1 1 calc R
H19B H 0.1757 0.2452 0.0871 0.163 Uiso 1 1 calc R
H19C H 0.1955 0.2132 0.1764 0.163 Uiso 1 1 calc R
C20 C 0.0976(3) 0.3592(8) 0.1712(6) 0.104(3) Uani 1 1 d .
H20A H 0.0780 0.3414 0.1189 0.157 Uiso 1 1 calc R
H20B H 0.0823 0.4206 0.1908 0.157 Uiso 1 1 calc R
H20C H 0.0977 0.2985 0.2058 0.157 Uiso 1 1 calc R
C21 C 0.2677(3) 0.5935(9) 0.1453(6) 0.111(3) Uani 1 1 d .
H21A H 0.2806 0.5328 0.1786 0.166 Uiso 1 1 calc R
H21B H 0.2575 0.6499 0.1765 0.166 Uiso 1 1 calc R
H21C H 0.2943 0.6200 0.1212 0.166 Uiso 1 1 calc R
C22 C 0.2345(4) 0.4563(8) -0.0016(7) 0.107(3) Uani 1 1 d .
H22A H 0.2055 0.4219 -0.0365 0.161 Uiso 1 1 calc R
H22B H 0.2563 0.4022 0.0290 0.161 Uiso 1 1 calc R
H22C H 0.2538 0.4965 -0.0322 0.161 Uiso 1 1 calc R
C23 C 0.1842(3) 0.6718(6) 0.0060(5) 0.080(2) Uani 1 1 d .
H23A H 0.1788 0.7291 0.0406 0.119 Uiso 1 1 calc R
H23B H 0.1519 0.6534 -0.0295 0.119 Uiso 1 1 calc R
H23C H 0.2082 0.6952 -0.0241 0.119 Uiso 1 1 calc R
N1 N -0.00324(18) 0.5325(4) 0.0905(3) 0.0456(11) Uani 1 1 d .
N2 N 0.04664(17) 0.7098(4) 0.0456(3) 0.0420(10) Uani 1 1 d .
N3 N 0.16170(18) 0.4970(4) 0.1017(3) 0.0488(11) Uani 1 1 d .
Nd1 Nd 0.077806(11) 0.54036(2) 0.040245(17) 0.04091(11) Uani 1 1 d .
Si1 Si 0.16599(7) 0.39283(16) 0.16746(11) 0.0611(5) Uani 1 1 d .
Si2 Si 0.21077(6) 0.55029(16) 0.06635(11) 0.0577(4) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 C1 C2 110.1(6) . .
N1 C1 Nd1 77.0(3) . 5_565
C2 C1 Nd1 78.0(4) . 5_565
C1 C2 C3 107.1(6) . .
C1 C2 Nd1 73.5(3) . 5_565
C3 C2 Nd1 78.4(4) . 5_565
C4 C3 C2 106.1(6) . .
C4 C3 Nd1 76.0(3) . 5_565
C2 C3 Nd1 73.2(4) . 5_565
N1 C4 C3 110.5(6) . .
N1 C4 C5 120.9(5) . .
C3 C4 C5 128.2(6) . .
N1 C4 Nd1 72.5(3) . 5_565
C3 C4 Nd1 76.2(3) . 5_565
C5 C4 Nd1 124.0(4) . 5_565
N2 C5 C4 112.3(5) . .
C11 C6 C7 119.5(5) . .
C11 C6 N2 119.8(5) . .
C7 C6 N2 120.7(5) . .
C8 C7 C6 119.1(6) . .
C8 C7 C12 119.5(6) . .
C6 C7 C12 121.4(6) . .
C9 C8 C7 121.1(7) . .
C10 C9 C8 120.4(7) . .
C9 C10 C11 121.2(7) . .
C10 C11 C6 118.6(6) . .
C10 C11 C15 119.3(6) . .
C6 C11 C15 122.0(5) . .
C7 C12 C14 112.6(7) . .
C7 C12 C13 111.6(6) . .
C14 C12 C13 110.2(6) . .
C17 C15 C16 108.5(7) . .
C17 C15 C11 113.8(7) . .
C16 C15 C11 110.7(6) . .
C4 N1 C1 106.2(5) . .
C4 N1 Nd1 110.3(3) . .
C1 N1 Nd1 142.5(4) . .
C4 N1 Nd1 79.7(3) . 5_565
C1 N1 Nd1 74.5(3) . 5_565
Nd1 N1 Nd1 103.62(15) . 5_565
C6 N2 C5 112.6(4) . .
C6 N2 Nd1 126.8(3) . .
C5 N2 Nd1 120.3(4) . .
Si2 N3 Si1 126.6(3) . .
Si2 N3 Nd1 119.1(3) . .
Si1 N3 Nd1 113.1(2) . .
N2 Nd1 N3 121.48(17) . .
N2 Nd1 N1 70.60(15) . .
N3 Nd1 N1 130.49(16) . .
N2 Nd1 C1 89.00(19) . 5_565
N3 Nd1 C1 126.87(18) . 5_565
N1 Nd1 C1 98.96(17) . 5_565
N2 Nd1 N1 97.68(15) . 5_565
N3 Nd1 N1 136.90(16) . 5_565
N1 Nd1 N1 76.38(15) . 5_565
C1 Nd1 N1 28.57(15) 5_565 5_565
N2 Nd1 C2 109.7(2) . 5_565
N3 Nd1 C2 98.6(2) . 5_565
N1 Nd1 C2 123.62(17) . 5_565
C1 Nd1 C2 28.5(2) 5_565 5_565
N1 Nd1 C2 47.29(16) 5_565 5_565
N2 Nd1 C4 125.42(17) . 5_565
N3 Nd1 C4 111.27(17) . 5_565
N1 Nd1 C4 86.35(15) . 5_565
C1 Nd1 C4 45.56(19) 5_565 5_565
N1 Nd1 C4 27.81(15) 5_565 5_565
C2 Nd1 C4 45.93(19) 5_565 5_565
N2 Nd1 C3 135.3(2) . 5_565
N3 Nd1 C3 90.29(19) . 5_565
N1 Nd1 C3 114.01(16) . 5_565
C1 Nd1 C3 46.5(2) 5_565 5_565
N1 Nd1 C3 46.84(17) 5_565 5_565
C2 Nd1 C3 28.4(2) 5_565 5_565
C4 Nd1 C3 27.75(16) 5_565 5_565
N3 Si1 C19 113.9(4) . .
N3 Si1 C18 114.7(4) . .
C19 Si1 C18 107.7(4) . .
N3 Si1 C20 106.0(3) . .
C19 Si1 C20 107.6(5) . .
C18 Si1 C20 106.5(4) . .
N3 Si2 C22 112.9(4) . .
N3 Si2 C21 114.0(4) . .
C22 Si2 C21 107.7(5) . .
N3 Si2 C23 106.9(3) . .
C22 Si2 C23 106.5(4) . .
C21 Si2 C23 108.5(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.370(7) .
C1 C2 1.373(10) .
C1 Nd1 2.760(6) 5_565
C2 C3 1.400(11) .
C2 Nd1 2.816(6) 5_565
C3 C4 1.382(8) .
C3 Nd1 2.883(6) 5_565
C4 N1 1.365(8) .
C4 C5 1.504(9) .
C4 Nd1 2.880(6) 5_565
C5 N2 1.451(7) .
C6 C11 1.398(8) .
C6 C7 1.404(8) .
C6 N2 1.427(7) .
C7 C8 1.381(9) .
C7 C12 1.510(9) .
C8 C9 1.359(12) .
C9 C10 1.356(12) .
C10 C11 1.393(9) .
C11 C15 1.527(9) .
C12 C14 1.521(10) .
C12 C13 1.535(10) .
C15 C17 1.496(10) .
C15 C16 1.514(12) .
C18 Si1 1.859(8) .
C19 Si1 1.844(9) .
C20 Si1 1.882(8) .
C21 Si2 1.867(9) .
C22 Si2 1.866(9) .
C23 Si2 1.871(8) .
N1 Nd1 2.511(4) .
N1 Nd1 2.791(5) 5_565
N2 Nd1 2.259(4) .
N3 Si2 1.701(5) .
N3 Si1 1.705(5) .
N3 Nd1 2.302(5) .
Nd1 C1 2.760(6) 5_565
Nd1 N1 2.791(5) 5_565
Nd1 C2 2.816(6) 5_565
Nd1 C4 2.880(6) 5_565
Nd1 C3 2.883(6) 5_565
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139160005
