#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:23:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179108 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/70/4307037.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_4307037
loop_
_publ_author_name
'You-gui Huang'
'Ben-lai Wu'
'Da-qiang Yuan'
'Yan-qing Xu'
'Fei-long Jiang'
'Mao-chun Hong'
_publ_section_title
;
New Lanthanide Hybrid as Clustered Infinite Nanotunnel with 3D Ln-O-Ln
Framework and (3,4)-Connected Net
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1171
_journal_page_last               1176
_journal_paper_doi               10.1021/ic0615271
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C28 H27 Dy3 N4 O24'
_chemical_formula_sum            'C28 H27 Dy3 N4 O24'
_chemical_formula_weight         1291.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                   14.9695(8)
_cell_length_b                   14.9695(8)
_cell_length_c                   14.6577(16)
_cell_measurement_reflns_used    3906
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.3451
_cell_volume                     3284.6(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2000)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Mercury CCD area-detector'
_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  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12316
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.35
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.868
_exptl_absorpt_correction_T_max  0.578
_exptl_absorpt_correction_T_min  0.263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2452
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.1800
_exptl_crystal_size_min          0.0800
_refine_diff_density_max         2.842
_refine_diff_density_min         -4.162
_refine_diff_density_rms         0.402
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.245
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.245
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.1038
_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)+(0.0000P)²+653.8235P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2388
_refine_ls_wR_factor_ref         0.2395
_reflns_number_gt                1857
_reflns_number_total             1883
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0615271si20060812_085514.cif
_cod_data_source_block           e:\data\hyg-1011\h
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4307037
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z+1/4'
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
Dy1 Dy 0.5000 0.2500 -0.1250 0.0252(5) Uani 1 4 d S . .
Dy2 Dy 0.30342(9) 0.02789(10) -0.14965(9) 0.0125(4) Uani 0.50 1 d P . .
O1 O 0.3473(11) 0.0697(12) 0.0051(11) 0.051(5) Uani 1 1 d . . .
O2 O 0.4157(9) 0.2040(9) 0.0015(8) 0.025(3) Uani 1 1 d . . .
O3 O 0.2292(11) 0.1111(9) 0.4456(10) 0.040(4) Uani 1 1 d . . .
O4 O 0.3116(11) 0.2326(12) 0.4668(9) 0.042(4) Uani 1 1 d . . .
O5 O 0.3694(10) 0.1688(9) -0.1803(9) 0.030(3) Uani 1 1 d . . .
O6 O 0.4620(14) -0.0198(12) -0.1114(12) 0.053(5) Uani 1 1 d . . .
N1 N 0.3073(10) 0.0893(10) 0.1823(9) 0.021(3) Uani 0.50 1 d P . .
N2 N 0.2843(10) 0.0968(11) 0.2698(10) 0.023(3) Uani 0.50 1 d P . .
C1 N 0.3073(10) 0.0893(10) 0.1823(9) 0.021(3) Uani 0.50 1 d P . .
C2 N 0.2843(10) 0.0968(11) 0.2698(10) 0.023(3) Uani 0.50 1 d P . .
C6 C 0.3742(11) 0.1418(12) 0.0405(11) 0.019(3) Uani 1 1 d . . .
C7 C 0.3545(10) 0.1542(11) 0.1409(9) 0.013(3) Uani 1 1 d . . .
C8 C 0.3838(11) 0.2285(10) 0.1902(11) 0.016(3) Uani 1 1 d . . .
H2 H 0.4166 0.2748 0.1611 0.020 Uiso 1 1 calc R . .
C3 C 0.3642(11) 0.2332(11) 0.2816(11) 0.017(3) Uani 1 1 d . . .
H3 H 0.3856 0.2816 0.3174 0.021 Uiso 1 1 calc R . .
C4 C 0.3135(10) 0.1676(10) 0.3205(10) 0.013(3) Uani 1 1 d . . .
C5 C 0.2819(12) 0.1723(13) 0.4195(12) 0.026(4) Uani 1 1 d . . .
H5 H 0.3759 0.1568 -0.1262 0.031 Uiso 1 1 d R . .
H6B H 0.4615 -0.0418 -0.0611 0.031 Uiso 1 1 d R . .
H6A H 0.4636 -0.0530 -0.1598 0.031 Uiso 1 1 d R . .
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'
Dy Dy -0.1892 4.4098 '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'
O O 0.0106 0.0060 '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'
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
_geom_angle_publ_flag
O2 Dy1 O2 128.6(4) 3_655 12_655 ?
O2 Dy1 O2 128.6(4) 3_655 10_665 ?
O2 Dy1 O2 75.6(6) 12_655 10_665 ?
O2 Dy1 O2 75.6(6) 3_655 . ?
O2 Dy1 O2 128.6(4) 12_655 . ?
O2 Dy1 O2 128.6(4) 10_665 . ?
O2 Dy1 O5 71.6(4) 3_655 3_655 ?
O2 Dy1 O5 76.7(5) 12_655 3_655 ?
O2 Dy1 O5 72.8(5) 10_665 3_655 ?
O2 Dy1 O5 147.1(4) . 3_655 ?
O2 Dy1 O5 147.1(4) 3_655 . ?
O2 Dy1 O5 72.8(5) 12_655 . ?
O2 Dy1 O5 76.7(5) 10_665 . ?
O2 Dy1 O5 71.6(4) . . ?
O5 Dy1 O5 141.2(6) 3_655 . ?
O2 Dy1 O5 72.8(5) 3_655 12_655 ?
O2 Dy1 O5 71.6(4) 12_655 12_655 ?
O2 Dy1 O5 147.1(4) 10_665 12_655 ?
O2 Dy1 O5 76.7(5) . 12_655 ?
O5 Dy1 O5 96.33(19) 3_655 12_655 ?
O5 Dy1 O5 96.33(19) . 12_655 ?
O2 Dy1 O5 76.7(5) 3_655 10_665 ?
O2 Dy1 O5 147.1(4) 12_655 10_665 ?
O2 Dy1 O5 71.6(4) 10_665 10_665 ?
O2 Dy1 O5 72.8(5) . 10_665 ?
O5 Dy1 O5 96.33(19) 3_655 10_665 ?
O5 Dy1 O5 96.33(19) . 10_665 ?
O5 Dy1 O5 141.2(6) 12_655 10_665 ?
O2 Dy1 H5 127.8 3_655 . ?
O2 Dy1 H5 84.6 12_655 . ?
O2 Dy1 H5 94.7 10_665 . ?
O2 Dy1 H5 53.1 . . ?
O5 Dy1 H5 159.6 3_655 . ?
O5 Dy1 H5 19.6 . . ?
O5 Dy1 H5 85.4 12_655 . ?
O5 Dy1 H5 94.9 10_665 . ?
O5 Dy2 O3 73.4(5) . 4_554 ?
O5 Dy2 O1 80.5(5) . . ?
O3 Dy2 O1 141.5(5) 4_554 . ?
O5 Dy2 C1 106.9(5) . 6_444 ?
O3 Dy2 C1 139.7(5) 4_554 6_444 ?
O1 Dy2 C1 74.8(5) . 6_444 ?
O5 Dy2 N1 106.9(5) . 6_444 ?
O3 Dy2 N1 139.7(5) 4_554 6_444 ?
O1 Dy2 N1 74.8(5) . 6_444 ?
C1 Dy2 N1 0.0(9) 6_444 6_444 ?
O5 Dy2 O1 80.5(6) . 6_444 ?
O3 Dy2 O1 76.2(5) 4_554 6_444 ?
O1 Dy2 O1 127.0(4) . 6_444 ?
C1 Dy2 O1 64.5(5) 6_444 6_444 ?
N1 Dy2 O1 64.5(5) 6_444 6_444 ?
O5 Dy2 O6 84.4(5) . . ?
O3 Dy2 O6 82.1(5) 4_554 . ?
O1 Dy2 O6 67.4(6) . . ?
C1 Dy2 O6 138.1(5) 6_444 . ?
N1 Dy2 O6 138.1(5) 6_444 . ?
O1 Dy2 O6 156.3(5) 6_444 . ?
O5 Dy2 O3 155.2(4) . 7_544 ?
O3 Dy2 O3 122.9(4) 4_554 7_544 ?
O1 Dy2 O3 75.7(5) . 7_544 ?
C1 Dy2 O3 73.5(5) 6_444 7_544 ?
N1 Dy2 O3 73.5(5) 6_444 7_544 ?
O1 Dy2 O3 119.7(5) 6_444 7_544 ?
O6 Dy2 O3 80.2(5) . 7_544 ?
O5 Dy2 C2 140.5(5) . 7_544 ?
O3 Dy2 C2 73.8(5) 4_554 7_544 ?
O1 Dy2 C2 138.6(5) . 7_544 ?
C1 Dy2 C2 84.9(5) 6_444 7_544 ?
N1 Dy2 C2 84.9(5) 6_444 7_544 ?
O1 Dy2 C2 70.9(6) 6_444 7_544 ?
O6 Dy2 C2 112.0(5) . 7_544 ?
O3 Dy2 C2 64.0(5) 7_544 7_544 ?
O5 Dy2 N2 140.5(5) . 7_544 ?
O3 Dy2 N2 73.8(5) 4_554 7_544 ?
O1 Dy2 N2 138.6(5) . 7_544 ?
C1 Dy2 N2 84.9(5) 6_444 7_544 ?
N1 Dy2 N2 84.9(5) 6_444 7_544 ?
O1 Dy2 N2 70.9(6) 6_444 7_544 ?
O6 Dy2 N2 112.0(5) . 7_544 ?
O3 Dy2 N2 64.0(5) 7_544 7_544 ?
C2 Dy2 N2 0.0(7) 7_544 7_544 ?
O5 Dy2 Dy2 82.2(3) . 6_444 ?
O3 Dy2 Dy2 40.0(4) 4_554 6_444 ?
O1 Dy2 Dy2 159.4(5) . 6_444 ?
C1 Dy2 Dy2 99.7(3) 6_444 6_444 ?
N1 Dy2 Dy2 99.7(3) 6_444 6_444 ?
O1 Dy2 Dy2 38.0(3) 6_444 6_444 ?
O6 Dy2 Dy2 121.9(4) . 6_444 ?
O3 Dy2 Dy2 122.5(3) 7_544 6_444 ?
C2 Dy2 Dy2 58.5(3) 7_544 6_444 ?
N2 Dy2 Dy2 58.5(3) 7_544 6_444 ?
O5 Dy2 Dy2 119.9(3) . 4 ?
O3 Dy2 Dy2 154.6(4) 4_554 4 ?
O1 Dy2 Dy2 39.7(4) . 4 ?
C1 Dy2 Dy2 61.0(3) 6_444 4 ?
N1 Dy2 Dy2 61.0(3) 6_444 4 ?
O1 Dy2 Dy2 125.2(3) 6_444 4 ?
O6 Dy2 Dy2 78.2(4) . 4 ?
O3 Dy2 Dy2 37.7(3) 7_544 4 ?
C2 Dy2 Dy2 99.0(3) 7_544 4 ?
N2 Dy2 Dy2 99.0(3) 7_544 4 ?
Dy2 Dy2 Dy2 153.11(4) 6_444 4 ?
O5 Dy2 H5 20.2 . . ?
O3 Dy2 H5 90.5 4_554 . ?
O1 Dy2 H5 60.4 . . ?
C1 Dy2 H5 100.9 6_444 . ?
N1 Dy2 H5 100.9 6_444 . ?
O1 Dy2 H5 94.8 6_444 . ?
O6 Dy2 H5 75.8 . . ?
O3 Dy2 H5 135.3 7_544 . ?
C2 Dy2 H5 160.7 7_544 . ?
N2 Dy2 H5 160.7 7_544 . ?
Dy2 Dy2 H5 102.2 6_444 . ?
Dy2 Dy2 H5 100.0 4 . ?
C6 O1 Dy2 133.3(15) . . ?
C6 O1 Dy2 121.7(12) . 4 ?
Dy2 O1 Dy2 102.4(5) . 4 ?
C6 O2 Dy1 147.4(11) . . ?
C5 O3 Dy2 124.4(14) . 6_445 ?
C5 O3 Dy2 122.9(12) . 7_545 ?
Dy2 O3 Dy2 102.3(5) 6_445 7_545 ?
Dy2 O5 Dy1 135.6(6) . . ?
Dy2 O5 H5 70.8 . . ?
Dy1 O5 H5 72.1 . . ?
Dy2 O6 H6B 107.9 . . ?
Dy2 O6 H6A 90.4 . . ?
H6B O6 H6A 120.8 . . ?
N2 N1 C7 120.5(14) . . ?
N2 N1 Dy2 119.5(11) . 4 ?
C7 N1 Dy2 119.7(10) . 4 ?
N1 N2 C4 120.5(14) . . ?
N1 N2 Dy2 120.8(11) . 7_545 ?
C4 N2 Dy2 118.5(10) . 7_545 ?
O2 C6 O1 127.2(16) . . ?
O2 C6 C7 116.6(14) . . ?
O1 C6 C7 116.3(16) . . ?
N1 C7 C8 120.5(13) . . ?
N1 C7 C6 116.9(14) . . ?
C8 C7 C6 122.7(14) . . ?
C3 C8 C7 118.5(15) . . ?
C3 C8 H2 120.7 . . ?
C7 C8 H2 120.7 . . ?
C4 C3 C8 119.3(15) . . ?
C4 C3 H3 120.4 . . ?
C8 C3 H3 120.4 . . ?
C3 C4 N2 120.6(14) . . ?
C3 C4 C5 122.3(15) . . ?
N2 C4 C5 117.0(15) . . ?
O4 C5 O3 126.0(17) . . ?
O4 C5 C4 117.4(17) . . ?
O3 C5 C4 116.5(18) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O2 2.347(12) 3_655 ?
Dy1 O2 2.347(12) 12_655 ?
Dy1 O2 2.347(12) 10_665 ?
Dy1 O2 2.347(12) . ?
Dy1 O5 2.440(13) 3_655 ?
Dy1 O5 2.440(13) . ?
Dy1 O5 2.440(13) 12_655 ?
Dy1 O5 2.440(13) 10_665 ?
Dy1 H5 2.3226 . ?
Dy2 O5 2.372(13) . ?
Dy2 O3 2.429(15) 4_554 ?
Dy2 O1 2.444(16) . ?
Dy2 C1 2.490(14) 6_444 ?
Dy2 N1 2.490(14) 6_444 ?
Dy2 O1 2.535(17) 6_444 ?
Dy2 O6 2.54(2) . ?
Dy2 O3 2.553(16) 7_544 ?
Dy2 C2 2.570(15) 7_544 ?
Dy2 N2 2.570(15) 7_544 ?
Dy2 Dy2 3.8802(8) 6_444 ?
Dy2 Dy2 3.8802(8) 4 ?
Dy2 H5 2.2409 . ?
O1 C6 1.26(2) . ?
O1 Dy2 2.535(17) 4 ?
O2 C6 1.26(2) . ?
O3 C5 1.27(2) . ?
O3 Dy2 2.429(15) 6_445 ?
O3 Dy2 2.553(16) 7_545 ?
O4 C5 1.22(3) . ?
O5 H5 0.8185 . ?
O6 H6B 0.8085 . ?
O6 H6A 0.8661 . ?
N1 N2 1.33(2) . ?
N1 C7 1.35(2) . ?
N1 Dy2 2.490(14) 4 ?
N2 C4 1.37(2) . ?
N2 Dy2 2.570(15) 7_545 ?
C6 C7 1.51(2) . ?
C7 C8 1.40(2) . ?
C8 C3 1.37(2) . ?
C8 H2 0.9500 . ?
C3 C4 1.37(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.53(2) . ?
