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#$Date: 2016-03-22 11:35:40 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178906 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/35/4113527.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_4113527
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 Dy N9 3+, 3 I 1-, 4(C2 H3 N)'
_chemical_formula_sum            'C26 H43 Dy I3 N13'
_chemical_formula_weight         1080.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.3218(3)
_cell_length_b                   13.8313(1)
_cell_length_c                   15.4992(1)
_cell_measurement_reflns_used    7779
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.62
_cell_measurement_theta_min      1.97
_cell_volume                     4356.47(8)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0740
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30673
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.872
_exptl_absorpt_correction_T_max  0.545187
_exptl_absorpt_correction_T_min  0.329393
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       block
_exptl_crystal_F_000             2060
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.831
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         4911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0419
_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)+(0.0482P)²+9.8274P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0995
_reflns_number_gt                4000
_reflns_number_total             4911
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja028311ssi20021230_025705_2.cif
_cod_data_source_block           Ib
_cod_database_code               4113527
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy Dy 0.425321(16) 0.2500 0.65016(2) 0.02068(10) Uani 1 2 d S . .
I1 I 0.653527(19) 0.48235(3) 0.61469(3) 0.03640(12) Uani 1 1 d . . .
I2 I 0.91018(3) 0.7500 0.70406(4) 0.03603(14) Uani 1 2 d S . .
N1 N 0.5444(3) 0.2500 0.6066(4) 0.0240(13) Uani 1 2 d S . .
H1A H 0.5647 0.3028 0.6276 0.080 Uiso 0.50 1 calc PR . .
H1B H 0.5647 0.1972 0.6276 0.080 Uiso 0.50 1 calc PR . .
N2 N 0.4561(2) 0.3564(3) 0.5303(3) 0.0221(9) Uani 1 1 d . . .
H2 H 0.4324 0.4065 0.5194 0.080 Uiso 1 1 calc R . .
C1 C 0.5470(3) 0.2500 0.5108(4) 0.0193(14) Uani 1 2 d S . .
C2 C 0.6168(4) 0.2500 0.4747(5) 0.0254(15) Uani 1 2 d S . .
H2A H 0.6398 0.3064 0.4947 0.080 Uiso 0.50 1 calc PR . .
H2B H 0.6152 0.2505 0.4128 0.080 Uiso 1 2 calc SR . .
H2C H 0.6396 0.1931 0.4940 0.080 Uiso 0.50 1 calc PR . .
C3 C 0.5067(2) 0.3390(3) 0.4838(3) 0.0194(10) Uani 1 1 d . . .
C4 C 0.5262(3) 0.3952(4) 0.4061(4) 0.0291(12) Uani 1 1 d . . .
H4A H 0.4927 0.4420 0.3932 0.080 Uiso 1 1 calc R . .
H4B H 0.5314 0.3522 0.3580 0.080 Uiso 1 1 calc R . .
H4C H 0.5670 0.4279 0.4170 0.080 Uiso 1 1 calc R . .
N3 N 0.3567(2) 0.4018(3) 0.6644(3) 0.0305(10) Uani 1 1 d . . .
C5 C 0.3240(3) 0.4685(4) 0.6665(4) 0.0317(12) Uani 1 1 d . . .
C6 C 0.2826(3) 0.5529(5) 0.6687(5) 0.0503(18) Uani 1 1 d . . .
H6A H 0.2697 0.5697 0.6111 0.080 Uiso 1 1 calc R . .
H6B H 0.3065 0.6058 0.6940 0.080 Uiso 1 1 calc R . .
H6C H 0.2442 0.5396 0.7026 0.080 Uiso 1 1 calc R . .
N4 N 0.4849(2) 0.3674(3) 0.7442(3) 0.0321(10) Uani 1 1 d . . .
C7 C 0.5080(3) 0.4315(4) 0.7784(4) 0.0294(12) Uani 1 1 d . . .
C8 C 0.5376(4) 0.5135(5) 0.8217(5) 0.0494(17) Uani 1 1 d . . .
H8A H 0.5302 0.5709 0.7883 0.080 Uiso 1 1 calc R . .
H8B H 0.5840 0.5029 0.8277 0.080 Uiso 1 1 calc R . .
H8C H 0.5181 0.5210 0.8778 0.080 Uiso 1 1 calc R . .
N5 N 0.3644(3) 0.2500 0.7928(4) 0.0329(15) Uani 1 2 d S . .
C9 C 0.3337(4) 0.2500 0.8535(6) 0.0368(19) Uani 1 2 d S . .
C10 C 0.2930(6) 0.2500 0.9304(7) 0.057(3) Uani 1 2 d S . .
H10A H 0.2671 0.3080 0.9319 0.080 Uiso 0.50 1 calc PR . .
H10B H 0.3206 0.2472 0.9806 0.080 Uiso 1 2 calc SR . .
H10C H 0.2644 0.1948 0.9294 0.080 Uiso 0.50 1 calc PR . .
N6 N 0.3328(3) 0.2500 0.5455(5) 0.0320(15) Uani 1 2 d S . .
C11 C 0.2976(4) 0.2500 0.4890(5) 0.0330(18) Uani 1 2 d S . .
C12 C 0.2516(5) 0.2500 0.4159(7) 0.054(3) Uani 1 2 d S . .
H12A H 0.2583 0.3071 0.3819 0.080 Uiso 0.50 1 calc PR . .
H12B H 0.2072 0.2491 0.4372 0.080 Uiso 1 2 calc SR . .
H12C H 0.2591 0.1938 0.3810 0.080 Uiso 0.50 1 calc PR . .
N7 N 0.1926(7) 0.7500 0.6542(8) 0.090(4) Uani 1 2 d S . .
C13 C 0.1526(6) 0.7500 0.7046(9) 0.060(3) Uani 1 2 d S . .
C14 C 0.1050(5) 0.7500 0.7735(9) 0.062(3) Uani 1 2 d S . .
H14A H 0.1137 0.6969 0.8118 0.080 Uiso 0.50 1 calc PR . .
H14B H 0.0616 0.7433 0.7498 0.080 Uiso 0.50 1 calc PR . .
H14C H 0.1079 0.8097 0.8049 0.080 Uiso 0.50 1 calc PR . .
N8 N 0.5384(8) 0.262(3) 0.9614(9) 0.103(6) Uiso 0.50 1 d P A -1
C15 C 0.4841(8) 0.3103(11) 0.9851(10) 0.059(4) Uiso 0.50 1 d P A -1
C16 C 0.4379(3) 0.3905(5) 0.9893(4) 0.117(8) Uiso 0.50 1 d P A -1
H16A H 0.4616 0.4505 0.9881 0.080 Uiso 0.50 1 calc PR A -1
H16B H 0.4129 0.3864 1.0418 0.080 Uiso 0.50 1 calc PR A -1
H16C H 0.4086 0.3876 0.9408 0.080 Uiso 0.50 1 calc PR A -1
N9 N 0.3315(3) 0.5884(6) 1.0665(4) 0.078(4) Uiso 0.50 1 d PR A -2
C17 C 0.3382(3) 0.5532(5) 0.9886(5) 0.064(4) Uiso 0.50 1 d PR A -2
C18 C 0.3457(4) 0.5132(5) 0.9089(4) 0.027(2) Uiso 0.50 1 d PR A -2
H18A H 0.3750 0.4589 0.9126 0.080 Uiso 0.50 1 calc PR A -2
H18B H 0.3636 0.5604 0.8701 0.080 Uiso 0.50 1 calc PR A -2
H18C H 0.3037 0.4919 0.8879 0.080 Uiso 0.50 1 calc PR A -2
N10 N 0.3241(3) 0.8678(5) 1.1084(5) 0.088(5) Uiso 0.50 1 d PR A -2
C19 C 0.3206(3) 0.8162(5) 1.1571(5) 0.057(4) Uiso 0.50 1 d PR A -2
C20 C 0.3117(3) 0.7445(6) 1.2188(4) 0.071(3) Uiso 0.50 1 d PR A -2
H20A H 0.2675 0.7204 1.2154 0.080 Uiso 0.50 1 calc PR A -2
H20B H 0.3193 0.7709 1.2752 0.080 Uiso 0.50 1 calc PR A -2
H20C H 0.3421 0.6926 1.2084 0.080 Uiso 0.50 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'
Dy Dy -0.1892 4.4098 '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
N2 Dy N2 73.82(19) 7_565 .
N2 Dy N6 72.46(16) 7_565 .
N2 Dy N6 72.46(16) . .
N2 Dy N4 135.18(15) 7_565 .
N2 Dy N4 85.88(15) . .
N6 Dy N4 138.52(11) . .
N2 Dy N4 85.88(15) 7_565 7_565
N2 Dy N4 135.17(15) . 7_565
N6 Dy N4 138.52(11) . 7_565
N4 Dy N4 81.1(2) . 7_565
N2 Dy N1 63.27(14) 7_565 .
N2 Dy N1 63.27(14) . .
N6 Dy N1 123.6(2) . .
N4 Dy N1 71.92(15) . .
N4 Dy N1 71.92(15) 7_565 .
N2 Dy N3 134.84(14) 7_565 .
N2 Dy N3 73.05(14) . .
N6 Dy N3 68.88(13) . .
N4 Dy N3 71.15(15) . .
N4 Dy N3 139.14(15) 7_565 .
N1 Dy N3 123.66(11) . .
N2 Dy N3 73.05(14) 7_565 7_565
N2 Dy N3 134.84(14) . 7_565
N6 Dy N3 68.88(13) . 7_565
N4 Dy N3 139.14(15) . 7_565
N4 Dy N3 71.15(15) 7_565 7_565
N1 Dy N3 123.66(11) . 7_565
N3 Dy N3 112.2(2) . 7_565
N2 Dy N5 141.80(10) 7_565 .
N2 Dy N5 141.80(10) . .
N6 Dy N5 101.5(2) . .
N4 Dy N5 74.19(16) . .
N4 Dy N5 74.19(16) 7_565 .
N1 Dy N5 134.9(2) . .
N3 Dy N5 69.80(13) . .
N3 Dy N5 69.80(13) 7_565 .
C1 N1 Dy 107.6(4) . .
C3 N2 Dy 121.3(3) . .
N1 C1 C2 113.6(6) . .
N1 C1 C3 104.7(4) . 7_565
C2 C1 C3 113.3(4) . 7_565
N1 C1 C3 104.7(4) . .
C2 C1 C3 113.3(4) . .
C3 C1 C3 106.5(5) 7_565 .
N2 C3 C4 124.9(4) . .
N2 C3 C1 115.2(4) . .
C4 C3 C1 119.9(5) . .
C5 N3 Dy 176.0(5) . .
N3 C5 C6 179.8(7) . .
C7 N4 Dy 169.1(4) . .
N4 C7 C8 179.8(8) . .
C9 N5 Dy 175.7(7) . .
N5 C9 C10 178.7(10) . .
C11 N6 Dy 170.0(7) . .
N6 C11 C12 179.7(10) . .
N7 C13 C14 176.0(15) . .
N8 C15 C16 158(2) . .
N9 C17 C18 177.8(3) . .
N10 C19 C20 175.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy N2 2.451(4) 7_565
Dy N2 2.451(4) .
Dy N6 2.483(7) .
Dy N4 2.496(5) .
Dy N4 2.496(5) 7_565
Dy N1 2.512(6) .
Dy N3 2.530(5) .
Dy N3 2.530(5) 7_565
Dy N5 2.534(7) .
N1 C1 1.485(9) .
N2 C3 1.279(6) .
C1 C2 1.526(9) .
C1 C3 1.536(6) 7_565
C1 C3 1.536(6) .
C3 C4 1.487(7) .
N3 C5 1.138(7) .
C5 C6 1.439(8) .
N4 C7 1.135(7) .
C7 C8 1.448(8) .
N5 C9 1.128(10) .
C9 C10 1.451(13) .
N6 C11 1.131(10) .
C11 C12 1.469(12) .
N7 C13 1.126(17) .
C13 C14 1.442(18) .
N8 C15 1.34(3) .
C15 C16 1.455(17) .
N9 C17 1.3082(18) .
C17 C18 1.3619(17) .
N10 C19 1.042(2) .
C19 C20 1.3891(19) .
