#------------------------------------------------------------------------------
#$Date: 2025-08-21 14:03:24 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301848 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/24/7022401.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_7022401
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 Si4 Sm2'
_chemical_formula_weight         1130.22
_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                 103.6210(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.5814(13)
_cell_length_b                   12.3473(6)
_cell_length_c                   17.3550(9)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.29
_cell_volume                     5535.9(5)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21076
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    2.221
_exptl_absorpt_correction_T_max  0.7040
_exptl_absorpt_correction_T_min  0.5652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            reddish
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5421
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0269P)²+5.7284P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0544
_refine_ls_wR_factor_ref         0.0588
_reflns_number_gt                4608
_reflns_number_total             5421
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32513f.txt
_cod_data_source_block           7b
_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               7022401
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 1.03393(13) 0.4624(3) 0.88133(18) 0.0562(8) Uani 1 1 d .
H1 H 1.0242 0.3936 0.8616 0.067 Uiso 1 1 calc R
C2 C 1.08183(14) 0.5087(3) 0.8854(2) 0.0667(10) Uani 1 1 d .
H2A H 1.1095 0.4772 0.8696 0.080 Uiso 1 1 calc R
C3 C 1.08064(12) 0.6116(3) 0.9178(2) 0.0631(9) Uani 1 1 d .
H3 H 1.1076 0.6616 0.9284 0.076 Uiso 1 1 calc R
C4 C 1.03152(11) 0.6254(2) 0.93106(18) 0.0496(7) Uani 1 1 d .
C5 C 1.00674(12) 0.7257(2) 0.9527(2) 0.0624(9) Uani 1 1 d .
H5A H 1.0258 0.7504 1.0044 0.075 Uiso 1 1 calc R
H5B H 1.0086 0.7821 0.9145 0.075 Uiso 1 1 calc R
C6 C 0.92386(10) 0.8073(2) 0.94491(16) 0.0425(6) Uani 1 1 d .
C7 C 0.92327(12) 0.8741(2) 1.00996(18) 0.0526(7) Uani 1 1 d .
C8 C 0.89187(17) 0.9651(3) 0.9989(3) 0.0780(11) Uani 1 1 d .
H8 H 0.8912 1.0095 1.0419 0.094 Uiso 1 1 calc R
C9 C 0.86202(18) 0.9908(3) 0.9263(3) 0.0917(14) Uani 1 1 d .
H9 H 0.8401 1.0505 0.9205 0.110 Uiso 1 1 calc R
C10 C 0.86416(15) 0.9289(3) 0.8619(2) 0.0761(11) Uani 1 1 d .
H10 H 0.8447 0.9491 0.8122 0.091 Uiso 1 1 calc R
C11 C 0.89472(12) 0.8365(2) 0.86888(19) 0.0534(7) Uani 1 1 d .
C12 C 0.95677(15) 0.8498(3) 1.09167(19) 0.0663(9) Uani 1 1 d .
H12 H 0.9754 0.7823 1.0876 0.080 Uiso 1 1 calc R
C13 C 0.99736(19) 0.9380(3) 1.1194(3) 0.0944(14) Uani 1 1 d .
H13A H 0.9804 1.0058 1.1230 0.142 Uiso 1 1 calc R
H13B H 1.0187 0.9446 1.0820 0.142 Uiso 1 1 calc R
H13C H 1.0185 0.9191 1.1704 0.142 Uiso 1 1 calc R
C14 C 0.92533(19) 0.8318(4) 1.1532(2) 0.0988(15) Uani 1 1 d .
H14A H 0.9018 0.7725 1.1369 0.148 Uiso 1 1 calc R
H14B H 0.9061 0.8962 1.1580 0.148 Uiso 1 1 calc R
H14C H 0.9482 0.8152 1.2034 0.148 Uiso 1 1 calc R
C15 C 0.89714(14) 0.7723(3) 0.79539(19) 0.0669(9) Uani 1 1 d .
H15 H 0.9180 0.7074 0.8121 0.080 Uiso 1 1 calc R
C16 C 0.9229(2) 0.8379(5) 0.7416(3) 0.159(3) Uani 1 1 d .
H16A H 0.9014 0.8986 0.7208 0.239 Uiso 1 1 calc R
H16B H 0.9278 0.7932 0.6987 0.239 Uiso 1 1 calc R
H16C H 0.9559 0.8634 0.7714 0.239 Uiso 1 1 calc R
C17 C 0.84538(18) 0.7374(4) 0.7476(3) 0.1170(18) Uani 1 1 d .
H17A H 0.8265 0.7996 0.7230 0.175 Uiso 1 1 calc R
H17B H 0.8265 0.7030 0.7816 0.175 Uiso 1 1 calc R
H17C H 0.8499 0.6873 0.7075 0.175 Uiso 1 1 calc R
C18 C 0.80050(18) 0.4273(4) 0.7299(2) 0.0886(12) Uani 1 1 d .
H18A H 0.8141 0.4935 0.7140 0.133 Uiso 1 1 calc R
H18B H 0.7642 0.4360 0.7273 0.133 Uiso 1 1 calc R
H18C H 0.8053 0.3698 0.6951 0.133 Uiso 1 1 calc R
C19 C 0.8052(2) 0.2695(3) 0.8625(3) 0.1066(16) Uani 1 1 d .
H19A H 0.7695 0.2831 0.8612 0.160 Uiso 1 1 calc R
H19B H 0.8231 0.2489 0.9152 0.160 Uiso 1 1 calc R
H19C H 0.8077 0.2120 0.8263 0.160 Uiso 1 1 calc R
C20 C 0.90329(16) 0.3582(4) 0.8293(3) 0.1076(17) Uani 1 1 d .
H20A H 0.9225 0.3373 0.8811 0.161 Uiso 1 1 calc R
H20B H 0.9195 0.4200 0.8117 0.161 Uiso 1 1 calc R
H20C H 0.9027 0.2993 0.7930 0.161 Uiso 1 1 calc R
C21 C 0.73375(15) 0.5931(4) 0.8551(3) 0.1075(16) Uani 1 1 d .
H21A H 0.7216 0.5326 0.8211 0.161 Uiso 1 1 calc R
H21B H 0.7438 0.6506 0.8246 0.161 Uiso 1 1 calc R
H21C H 0.7066 0.6180 0.8787 0.161 Uiso 1 1 calc R
C22 C 0.76629(19) 0.4568(4) 1.0018(3) 0.1037(16) Uani 1 1 d .
H22A H 0.7950 0.4317 1.0424 0.156 Uiso 1 1 calc R
H22B H 0.7494 0.3960 0.9720 0.156 Uiso 1 1 calc R
H22C H 0.7422 0.4942 1.0257 0.156 Uiso 1 1 calc R
C23 C 0.81568(14) 0.6743(3) 0.9935(2) 0.0781(11) Uani 1 1 d .
H23A H 0.8207 0.7313 0.9585 0.117 Uiso 1 1 calc R
H23B H 0.8481 0.6573 1.0294 0.117 Uiso 1 1 calc R
H23C H 0.7913 0.6973 1.0231 0.117 Uiso 1 1 calc R
N1 N 1.00276(9) 0.53215(18) 0.91049(14) 0.0454(6) Uani 1 1 d .
N2 N 0.95269(8) 0.70853(17) 0.95439(13) 0.0422(5) Uani 1 1 d .
N3 N 0.83965(9) 0.4978(2) 0.89882(14) 0.0465(5) Uani 1 1 d .
Si1 Si 0.83506(4) 0.39378(8) 0.83314(6) 0.0598(2) Uani 1 1 d .
Si2 Si 0.79019(3) 0.55112(7) 0.93397(6) 0.0567(2) Uani 1 1 d .
Sm1 Sm 0.922882(5) 0.540192(11) 0.959851(8) 0.03866(6) 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'
Sm Sm -0.1638 3.4418 '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'
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 110.5(3) . .
N1 C1 Sm1 77.37(16) . 5_767
C2 C1 Sm1 77.8(2) . 5_767
C1 C2 C3 106.9(3) . .
C1 C2 Sm1 73.14(18) . 5_767
C3 C2 Sm1 78.39(19) . 5_767
C4 C3 C2 106.9(3) . .
C4 C3 Sm1 76.10(16) . 5_767
C2 C3 Sm1 73.02(18) . 5_767
N1 C4 C3 109.8(3) . .
N1 C4 C5 120.5(2) . .
C3 C4 C5 129.2(3) . .
N1 C4 Sm1 72.37(14) . 5_767
C3 C4 Sm1 75.72(17) . 5_767
C5 C4 Sm1 124.9(2) . 5_767
N2 C5 C4 112.3(2) . .
C7 C6 C11 119.7(3) . .
C7 C6 N2 121.1(3) . .
C11 C6 N2 119.2(2) . .
C8 C7 C6 119.1(3) . .
C8 C7 C12 119.5(3) . .
C6 C7 C12 121.4(3) . .
C9 C8 C7 121.3(4) . .
C8 C9 C10 120.0(4) . .
C9 C10 C11 121.6(4) . .
C10 C11 C6 118.2(3) . .
C10 C11 C15 119.7(3) . .
C6 C11 C15 122.1(3) . .
C7 C12 C14 112.8(3) . .
C7 C12 C13 111.6(3) . .
C14 C12 C13 110.4(3) . .
C17 C15 C11 113.7(3) . .
C17 C15 C16 107.7(4) . .
C11 C15 C16 110.7(3) . .
C1 N1 C4 105.9(3) . .
C1 N1 Sm1 142.7(2) . .
C4 N1 Sm1 110.19(17) . .
C1 N1 Sm1 73.73(16) . 5_767
C4 N1 Sm1 79.25(16) . 5_767
Sm1 N1 Sm1 103.78(8) . 5_767
C6 N2 C5 112.2(2) . .
C6 N2 Sm1 127.79(17) . .
C5 N2 Sm1 119.79(17) . .
Si1 N3 Si2 126.21(15) . .
Si1 N3 Sm1 113.18(12) . .
Si2 N3 Sm1 119.39(13) . .
N3 Si1 C19 114.12(18) . .
N3 Si1 C18 114.77(17) . .
C19 Si1 C18 107.7(2) . .
N3 Si1 C20 106.38(16) . .
C19 Si1 C20 107.1(2) . .
C18 Si1 C20 106.2(2) . .
N3 Si1 Sm1 38.86(8) . .
C19 Si1 Sm1 123.07(15) . .
C18 Si1 Sm1 128.69(14) . .
C20 Si1 Sm1 67.64(13) . .
N3 Si2 C21 113.73(18) . .
N3 Si2 C22 112.89(17) . .
C21 Si2 C22 107.7(2) . .
N3 Si2 C23 107.54(15) . .
C21 Si2 C23 107.8(2) . .
C22 Si2 C23 106.9(2) . .
N3 Si2 Sm1 35.09(8) . .
C21 Si2 Sm1 137.11(17) . .
C22 Si2 Sm1 112.45(17) . .
C23 Si2 Sm1 74.58(11) . .
N2 Sm1 N3 120.64(8) . .
N2 Sm1 N1 71.37(8) . .
N3 Sm1 N1 130.49(8) . .
N2 Sm1 C1 89.12(9) . 5_767
N3 Sm1 C1 126.83(9) . 5_767
N1 Sm1 C1 99.11(9) . 5_767
N2 Sm1 N1 98.17(8) . 5_767
N3 Sm1 N1 137.12(8) . 5_767
N1 Sm1 N1 76.22(8) . 5_767
C1 Sm1 N1 28.89(7) 5_767 5_767
N2 Sm1 C2 109.85(11) . 5_767
N3 Sm1 C2 98.01(10) . 5_767
N1 Sm1 C2 124.27(9) . 5_767
C1 Sm1 C2 29.04(10) 5_767 5_767
N1 Sm1 C2 48.09(8) 5_767 5_767
N2 Sm1 C3 135.84(10) . 5_767
N3 Sm1 C3 89.80(9) . 5_767
N1 Sm1 C3 114.42(8) . 5_767
C1 Sm1 C3 47.05(11) 5_767 5_767
N1 Sm1 C3 47.55(8) 5_767 5_767
C2 Sm1 C3 28.58(11) 5_767 5_767
N2 Sm1 C4 126.50(9) . 5_767
N3 Sm1 C4 110.97(9) . 5_767
N1 Sm1 C4 86.32(8) . 5_767
C1 Sm1 C4 46.29(10) 5_767 5_767
N1 Sm1 C4 28.38(8) 5_767 5_767
C2 Sm1 C4 46.65(9) 5_767 5_767
C3 Sm1 C4 28.17(8) 5_767 5_767
N2 Sm1 Si1 132.53(6) . .
N3 Sm1 Si1 27.96(6) . .
N1 Sm1 Si1 105.94(6) . .
C1 Sm1 Si1 136.29(8) 5_767 .
N1 Sm1 Si1 127.97(5) 5_767 .
C2 Sm1 Si1 109.56(9) 5_767 .
C3 Sm1 Si1 89.67(8) 5_767 .
C4 Sm1 Si1 99.84(7) 5_767 .
N2 Sm1 Si2 108.65(6) . .
N3 Sm1 Si2 25.52(6) . .
N1 Sm1 Si2 153.05(6) . .
C1 Sm1 Si2 107.84(7) 5_767 .
N1 Sm1 Si2 129.06(5) 5_767 .
C2 Sm1 Si2 81.80(7) 5_767 .
C3 Sm1 Si2 84.89(6) 5_767 .
C4 Sm1 Si2 112.06(6) 5_767 .
Si1 Sm1 Si2 53.17(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.372(4) .
C1 C2 1.382(5) .
C1 Sm1 2.725(3) 5_767
C2 C3 1.392(5) .
C2 Sm1 2.783(3) 5_767
C3 C4 1.389(4) .
C3 Sm1 2.851(3) 5_767
C4 N1 1.382(4) .
C4 C5 1.492(4) .
C4 Sm1 2.855(3) 5_767
C5 N2 1.460(4) .
C6 C7 1.402(4) .
C6 C11 1.411(4) .
C6 N2 1.429(3) .
C7 C8 1.385(5) .
C7 C12 1.516(5) .
C8 C9 1.358(6) .
C9 C10 1.367(6) .
C10 C11 1.389(4) .
C11 C15 1.516(4) .
C12 C14 1.519(5) .
C12 C13 1.529(5) .
C15 C17 1.493(5) .
C15 C16 1.516(6) .
C18 Si1 1.857(4) .
C19 Si1 1.853(4) .
C20 Si1 1.883(4) .
C21 Si2 1.851(4) .
C22 Si2 1.870(4) .
C23 Si2 1.873(4) .
N1 Sm1 2.472(2) .
N1 Sm1 2.770(2) 5_767
N2 Sm1 2.234(2) .
N3 Si1 1.702(3) .
N3 Si2 1.707(2) .
N3 Sm1 2.278(2) .
Si1 Sm1 3.3371(9) .
Si2 Sm1 3.4518(9) .
Sm1 C1 2.725(3) 5_767
Sm1 N1 2.770(2) 5_767
Sm1 C2 2.783(3) 5_767
Sm1 C3 2.851(3) 5_767
Sm1 C4 2.855(3) 5_767
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139160006
