#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:35:40 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178906 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/35/4113526.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_4113526
loop_
_publ_author_name
'Mikhail N. Bochkarev'
'Georgii V. Khoroshenkov'
'Herbert Schumann'
'Sebastian Dechert'
_publ_contact_author_address
; Razuvaev Institute of Organometallic Chemistry 
  Russian Academy of Sciences 
  Tropinina 49  
  603950 Nizhny Novgorod
  Russia 
;
_publ_contact_author_email       mboch@imoc.sinn.ru
_publ_contact_author_fax         (8312)66-67-95
_publ_contact_author_name        'Prof. Dr. M. N. Bochkarev'
_publ_contact_author_phone       (8312)66-14-97
_publ_section_title
;
 A Novel Bis(imino)amine Ligand as a Result of Acetonitrile Coupling with
 the Diiodides of Dy(II) and Tm(II)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2894
_journal_page_last               2895
_journal_paper_doi               10.1021/ja028311s
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C18 H31 N9 Tm 3+, 3 I 1-, 2(C2 H3 N)'
_chemical_formula_sum            'C22 H37 I3 N11 Tm'
_chemical_formula_weight         1005.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                69.641(1)
_cell_angle_beta                 89.732(1)
_cell_angle_gamma                73.989(1)
_cell_formula_units_Z            2
_cell_length_a                   10.7188(3)
_cell_length_b                   13.7619(5)
_cell_length_c                   14.0021(5)
_cell_measurement_reflns_used    3647
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.55
_cell_measurement_theta_min      1.56
_cell_volume                     1851.75(11)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'ZORTEP (Zsolnai, Pritzkow, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       ω
_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  0.0501
_diffrn_reflns_av_sigmaI/netI    0.0988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12405
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.923
_exptl_absorpt_correction_T_max  0.694916
_exptl_absorpt_correction_T_min  0.437734
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_description       'irregular shape'
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.931
_refine_diff_density_min         -1.521
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         7169
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0283P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1061
_reflns_number_gt                5054
_reflns_number_total             7169
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja028311ssi20021230_025705_1.cif
_cod_data_source_block           Ic
_cod_database_code               4113526
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Tm Tm 0.84081(3) 0.36908(3) 0.29679(3) 0.01939(11) Uani 1 1 d . . .
I1 I 0.71338(6) 0.70638(5) -0.08900(5) 0.03748(18) Uani 1 1 d . . .
I2 I 1.17123(6) 0.82273(5) 0.14911(5) 0.03582(17) Uani 1 1 d . . .
I3 I 0.70549(6) 0.73226(6) 0.43436(5) 0.04392(19) Uani 1 1 d . . .
N1 N 1.0793(6) 0.3489(5) 0.3079(5) 0.0220(16) Uani 1 1 d . . .
H1A H 1.1149 0.3137 0.3732 0.080 Uiso 1 1 calc R . .
H1B H 1.1195 0.3109 0.2699 0.080 Uiso 1 1 calc R . .
N2 N 0.9096(6) 0.4910(5) 0.3614(5) 0.0227(16) Uani 1 1 d . . .
H2 H 0.8637 0.5164 0.4026 0.080 Uiso 1 1 calc R . .
N3 N 0.9143(6) 0.4896(5) 0.1505(5) 0.0220(16) Uani 1 1 d . . .
H3 H 0.8710 0.5149 0.0912 0.080 Uiso 1 1 calc R . .
N4 N 0.7129(7) 0.3845(6) 0.4449(6) 0.0282(17) Uani 1 1 d . . .
N5 N 0.9464(7) 0.2161(6) 0.4518(6) 0.0312(18) Uani 1 1 d . . .
N6 N 0.6948(7) 0.2524(6) 0.3346(6) 0.0319(18) Uani 1 1 d . . .
N7 N 0.6651(7) 0.5437(6) 0.2372(6) 0.0293(18) Uani 1 1 d . . .
N8 N 0.7135(7) 0.3897(6) 0.1375(6) 0.0254(17) Uani 1 1 d . . .
N9 N 0.9443(7) 0.2300(6) 0.2297(6) 0.0288(17) Uani 1 1 d . . .
C1 C 1.0939(7) 0.4605(6) 0.2684(6) 0.0201(18) Uani 1 1 d . . .
C2 C 1.2356(8) 0.4622(8) 0.2694(7) 0.034(2) Uani 1 1 d . . .
H2A H 1.2780 0.4242 0.3378 0.080 Uiso 1 1 calc R . .
H2B H 1.2383 0.5358 0.2464 0.080 Uiso 1 1 calc R . .
H2C H 1.2796 0.4275 0.2248 0.080 Uiso 1 1 calc R . .
C3 C 1.0123(8) 0.5174(7) 0.3350(6) 0.0246(19) Uani 1 1 d . . .
C4 C 1.0566(9) 0.5986(8) 0.3632(7) 0.036(2) Uani 1 1 d . . .
H4A H 0.9890 0.6355 0.3944 0.080 Uiso 1 1 calc R . .
H4B H 1.0754 0.6503 0.3027 0.080 Uiso 1 1 calc R . .
H4C H 1.1338 0.5623 0.4106 0.080 Uiso 1 1 calc R . .
C5 C 1.0165(8) 0.5147(6) 0.1620(6) 0.0218(19) Uani 1 1 d . . .
C6 C 1.0627(9) 0.5965(7) 0.0777(7) 0.031(2) Uani 1 1 d . . .
H6A H 1.0071 0.6201 0.0155 0.080 Uiso 1 1 calc R . .
H6B H 1.1506 0.5637 0.0674 0.080 Uiso 1 1 calc R . .
H6C H 1.0599 0.6576 0.0968 0.080 Uiso 1 1 calc R . .
C7 C 0.6623(8) 0.3815(7) 0.5141(7) 0.027(2) Uani 1 1 d . . .
C8 C 0.5932(9) 0.3776(9) 0.6072(7) 0.040(3) Uani 1 1 d . . .
H8A H 0.5654 0.4488 0.6106 0.080 Uiso 1 1 calc R . .
H8B H 0.6511 0.3287 0.6670 0.080 Uiso 1 1 calc R . .
H8C H 0.5185 0.3528 0.6040 0.080 Uiso 1 1 calc R . .
C9 C 0.9998(9) 0.1461(8) 0.5253(7) 0.038(2) Uani 1 1 d . . .
C10 C 1.0667(12) 0.0601(9) 0.6162(8) 0.065(4) Uani 1 1 d . . .
H10A H 1.1305 0.0821 0.6449 0.080 Uiso 1 1 calc R . .
H10B H 1.1094 -0.0026 0.6001 0.080 Uiso 1 1 calc R . .
H10C H 1.0053 0.0430 0.6648 0.080 Uiso 1 1 calc R . .
C11 C 0.6225(9) 0.2040(8) 0.3490(7) 0.030(2) Uani 1 1 d . . .
C12 C 0.5250(10) 0.1426(8) 0.3675(8) 0.046(3) Uani 1 1 d . . .
H12A H 0.4780 0.1522 0.4237 0.080 Uiso 1 1 calc R . .
H12B H 0.5689 0.0670 0.3837 0.080 Uiso 1 1 calc R . .
H12C H 0.4651 0.1689 0.3072 0.080 Uiso 1 1 calc R . .
C13 C 0.6169(8) 0.6346(8) 0.2045(7) 0.030(2) Uani 1 1 d . . .
C14 C 0.5563(9) 0.7526(7) 0.1579(8) 0.040(2) Uani 1 1 d . . .
H14A H 0.5774 0.7783 0.0886 0.080 Uiso 1 1 calc R . .
H14B H 0.5885 0.7879 0.1963 0.080 Uiso 1 1 calc R . .
H14C H 0.4633 0.7685 0.1583 0.080 Uiso 1 1 calc R . .
C15 C 0.6638(8) 0.3853(7) 0.0701(7) 0.029(2) Uani 1 1 d . . .
C16 C 0.6020(9) 0.3779(10) -0.0184(8) 0.046(3) Uani 1 1 d . . .
H16A H 0.6564 0.3185 -0.0343 0.080 Uiso 1 1 calc R . .
H16B H 0.5903 0.4441 -0.0759 0.080 Uiso 1 1 calc R . .
H16C H 0.5187 0.3663 -0.0033 0.080 Uiso 1 1 calc R . .
C17 C 0.9881(8) 0.1816(7) 0.1795(7) 0.029(2) Uani 1 1 d . . .
C18 C 1.0400(10) 0.1225(8) 0.1131(8) 0.045(3) Uani 1 1 d . . .
H18A H 1.0650 0.0461 0.1519 0.080 Uiso 1 1 calc R . .
H18B H 1.1148 0.1429 0.0849 0.080 Uiso 1 1 calc R . .
H18C H 0.9745 0.1395 0.0585 0.080 Uiso 1 1 calc R . .
N10 N 0.2303(14) 0.0056(12) 0.4131(12) 0.110(5) Uani 1 1 d . . .
C19 C 0.2908(14) -0.0088(11) 0.3544(12) 0.065(4) Uani 1 1 d . . .
C20 C 0.3722(12) -0.0281(9) 0.2748(10) 0.069(4) Uani 1 1 d . . .
H20A H 0.3771 0.0399 0.2266 0.080 Uiso 1 1 calc R . .
H20B H 0.3347 -0.0641 0.2401 0.080 Uiso 1 1 calc R . .
H20C H 0.4583 -0.0728 0.3056 0.080 Uiso 1 1 calc R . .
N11A N 0.686(3) 0.084(3) 0.169(3) 0.184(17) Uiso 0.67(2) 1 d PD A 1
C21A C 0.762(3) 0.007(3) 0.154(3) 0.149(16) Uiso 0.67(2) 1 d PD A 1
C22A C 0.7726(17) -0.0613(13) 0.1035(13) 0.049(5) Uiso 0.67(2) 1 d PD A 1
H22A H 0.7807 -0.1328 0.1515 0.080 Uiso 0.67(2) 1 calc PR A 1
H22B H 0.8485 -0.0624 0.0667 0.080 Uiso 0.67(2) 1 calc PR A 1
H22C H 0.6963 -0.0375 0.0562 0.080 Uiso 0.67(2) 1 calc PR A 1
N11B N 0.710(3) 0.105(2) 0.169(2) 0.034(8) Uiso 0.33(2) 1 d PD A 2
C21B C 0.724(3) 0.034(2) 0.1317(19) 0.013(6) Uiso 0.33(2) 1 d PD A 2
C22B C 0.660(5) -0.007(4) 0.081(4) 0.12(2) Uiso 0.33(2) 1 d PD A 2
H22D H 0.6383 -0.0675 0.1284 0.080 Uiso 0.33(2) 1 calc PR A 2
H22E H 0.7146 -0.0294 0.0333 0.080 Uiso 0.33(2) 1 calc PR A 2
H22F H 0.5817 0.0480 0.0440 0.080 Uiso 0.33(2) 1 calc PR A 2
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 '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
N9 Tm N3 84.9(2)
N9 Tm N2 136.5(2)
N3 Tm N2 75.0(2)
N9 Tm N5 77.7(3)
N3 Tm N5 135.6(2)
N2 Tm N5 90.2(2)
N9 Tm N6 76.9(2)
N3 Tm N6 139.7(2)
N2 Tm N6 140.3(2)
N5 Tm N6 75.1(2)
N9 Tm N7 137.3(3)
N3 Tm N7 73.7(2)
N2 Tm N7 73.0(2)
N5 Tm N7 141.9(2)
N6 Tm N7 96.1(2)
N9 Tm N1 73.0(2)
N3 Tm N1 64.5(2)
N2 Tm N1 63.6(2)
N5 Tm N1 71.3(2)
N6 Tm N1 138.6(2)
N7 Tm N1 125.3(2)
N9 Tm N8 68.4(2)
N3 Tm N8 71.7(2)
N2 Tm N8 135.4(2)
N5 Tm N8 134.4(2)
N6 Tm N8 68.3(2)
N7 Tm N8 69.9(2)
N1 Tm N8 123.0(2)
N9 Tm N4 137.9(2)
N3 Tm N4 137.2(2)
N2 Tm N4 71.8(2)
N5 Tm N4 71.0(2)
N6 Tm N4 68.5(2)
N7 Tm N4 71.3(2)
N1 Tm N4 120.1(2)
N8 Tm N4 116.7(2)
C1 N1 Tm 107.0(4)
C3 N2 Tm 120.6(6)
C5 N3 Tm 119.6(5)
C7 N4 Tm 173.6(7)
C9 N5 Tm 177.2(8)
C11 N6 Tm 176.2(8)
C13 N7 Tm 159.2(7)
C15 N8 Tm 171.2(7)
C17 N9 Tm 166.1(7)
N1 C1 C2 113.5(7)
N1 C1 C5 104.7(6)
C2 C1 C5 114.6(7)
N1 C1 C3 104.2(6)
C2 C1 C3 114.0(7)
C5 C1 C3 104.7(6)
N2 C3 C4 124.7(8)
N2 C3 C1 115.8(8)
C4 C3 C1 119.5(7)
N3 C5 C6 123.2(8)
N3 C5 C1 117.3(7)
C6 C5 C1 119.4(7)
N4 C7 C8 179.6(10)
N5 C9 C10 179.4(12)
N6 C11 C12 178.7(11)
N7 C13 C14 177.6(10)
N8 C15 C16 178.5(10)
N9 C17 C18 178.0(10)
N10 C19 C20 180(2)
N11A C21A C22A 143(3)
N11B C21B C22B 143(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Tm N9 2.419(8)
Tm N3 2.431(6)
Tm N2 2.434(7)
Tm N5 2.440(7)
Tm N6 2.469(8)
Tm N7 2.478(7)
Tm N1 2.493(6)
Tm N8 2.508(8)
Tm N4 2.519(7)
N1 C1 1.493(10)
N2 C3 1.267(10)
N3 C5 1.262(10)
N4 C7 1.102(10)
N5 C9 1.152(11)
N6 C11 1.129(11)
N7 C13 1.134(11)
N8 C15 1.114(11)
N9 C17 1.143(11)
C1 C2 1.525(11)
C1 C5 1.537(11)
C1 C3 1.540(12)
C3 C4 1.494(12)
C5 C6 1.511(10)
C7 C8 1.488(12)
C9 C10 1.423(13)
C11 C12 1.485(12)
C13 C14 1.473(13)
C15 C16 1.455(13)
C17 C18 1.452(14)
N10 C19 1.084(17)
C19 C20 1.463(18)
N11A C21A 1.23(2)
C21A C22A 1.34(3)
N11B C21B 1.23(2)
C21B C22B 1.34(3)
