#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/44/7104453.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_7104453
loop_
_publ_author_name
'Zhao, Bin'
'Chen, Xiao-Yan'
'Chen, Zhi'
'Shi, Wei'
'Cheng, Peng'
'Yan, Shi-Ping'
'Liao, Dai-Zheng'
_publ_section_title
;
 A porous 3D heterometal-organic framework containing both lanthanide
 and high-spin Fe(ii) ions.
;
_journal_issue                   21
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3113
_journal_page_last               3115
_journal_paper_doi               10.1039/b821496d
_journal_volume                  34
_journal_year                    2009
_chemical_formula_sum            'C21 H18 Fe1.5 N3 O16.5 Tb'
_chemical_formula_weight         819.08
_chemical_name_systematic
;
?
;
_space_group_IT_number           192
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6 2c'
_symmetry_space_group_name_H-M   'P 6/m c c'
_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                120.00
_cell_formula_units_Z            4
_cell_length_a                   15.199(2)
_cell_length_b                   15.199(2)
_cell_length_c                   15.589(5)
_cell_measurement_reflns_used    881
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.33
_cell_measurement_theta_min      3.04
_cell_volume                     3118.8(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0550
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11486
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    3.012
_exptl_absorpt_correction_T_max  0.8890
_exptl_absorpt_correction_T_min  0.7527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.054
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0256
_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)+(0.0349P)²+7.7317P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0742
_reflns_number_gt                707
_reflns_number_total             948
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b821496d.txt
_cod_data_source_block           030109b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_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.

'_refine_ls_hydrogen_treatment' value 'CONSTR' changed to
'constr' 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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'NONE' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P6/mcc
_cod_original_formula_sum        'C21 H18 Fe1.50 N3 O16.50 Tb'
_cod_database_code               7104453
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, 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
Tb1 Tb 0.3333 0.6667 0.2500 0.01860(18) Uani 1 6 d S . .
Fe1 Fe 0.5000 0.5000 0.0000 0.0186(3) Uani 1 4 d S . .
O1 O 0.4136(2) 0.6125(2) 0.14348(19) 0.0287(7) Uani 1 1 d . . .
O2 O 0.5521(3) 0.6152(3) 0.0920(2) 0.0378(9) Uani 1 1 d . . .
O3 O 0.6505(3) 0.5127(4) 0.0000 0.0287(11) Uani 1 2 d S . .
N1 N 0.5222(4) 0.76111(18) 0.2500 0.0221(10) Uani 1 2 d S . .
C1 C 0.7306(5) 0.8653(3) 0.2500 0.053(2) Uani 1 2 d S . .
H1 H 0.8013 0.9006 0.2500 0.064 Uiso 1 2 calc SR . .
C2 C 0.6778(4) 0.7863(4) 0.1940(4) 0.0398(13) Uani 1 1 d . . .
H2 H 0.7121 0.7676 0.1553 0.048 Uiso 1 1 calc R . .
C3 C 0.5736(3) 0.7353(3) 0.1961(3) 0.0265(10) Uani 1 1 d . . .
C4 C 0.5082(4) 0.6471(4) 0.1388(3) 0.0265(10) Uani 1 1 d . . .
O4 O 0.7879(13) 0.7391(12) 0.0000 0.103(7) Uani 0.50 2 d SP . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 '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
O1 Tb1 O1 145.94(15) 3_565 12_565 ?
O1 Tb1 O1 86.78(15) 3_565 11 ?
O1 Tb1 O1 78.58(11) 12_565 11 ?
O1 Tb1 O1 78.58(11) 3_565 2_665 ?
O1 Tb1 O1 86.78(15) 12_565 2_665 ?
O1 Tb1 O1 128.58(15) 11 2_665 ?
O1 Tb1 O1 78.58(11) 3_565 . ?
O1 Tb1 O1 128.58(15) 12_565 . ?
O1 Tb1 O1 145.94(15) 11 . ?
O1 Tb1 O1 78.58(11) 2_665 . ?
O1 Tb1 O1 128.58(15) 3_565 10_665 ?
O1 Tb1 O1 78.58(11) 12_565 10_665 ?
O1 Tb1 O1 78.58(11) 11 10_665 ?
O1 Tb1 O1 145.94(15) 2_665 10_665 ?
O1 Tb1 O1 86.78(15) . 10_665 ?
O1 Tb1 N1 72.97(7) 3_565 2_665 ?
O1 Tb1 N1 72.97(7) 12_565 2_665 ?
O1 Tb1 N1 64.29(7) 11 2_665 ?
O1 Tb1 N1 64.29(7) 2_665 2_665 ?
O1 Tb1 N1 136.61(7) . 2_665 ?
O1 Tb1 N1 136.61(7) 10_665 2_665 ?
O1 Tb1 N1 64.29(7) 3_565 3_565 ?
O1 Tb1 N1 136.61(7) 12_565 3_565 ?
O1 Tb1 N1 72.97(7) 11 3_565 ?
O1 Tb1 N1 136.61(7) 2_665 3_565 ?
O1 Tb1 N1 72.97(7) . 3_565 ?
O1 Tb1 N1 64.29(7) 10_665 3_565 ?
N1 Tb1 N1 120.0 2_665 3_565 ?
O1 Tb1 N1 136.61(7) 3_565 . ?
O1 Tb1 N1 64.29(7) 12_565 . ?
O1 Tb1 N1 136.61(7) 11 . ?
O1 Tb1 N1 72.97(7) 2_665 . ?
O1 Tb1 N1 64.29(7) . . ?
O1 Tb1 N1 72.97(7) 10_665 . ?
N1 Tb1 N1 120.0 2_665 . ?
N1 Tb1 N1 120.0 3_565 . ?
O2 Fe1 O2 180.0 . 13_665 ?
O2 Fe1 O2 86.7(2) . 16 ?
O2 Fe1 O2 93.3(2) 13_665 16 ?
O2 Fe1 O2 93.3(2) . 4_665 ?
O2 Fe1 O2 86.7(2) 13_665 4_665 ?
O2 Fe1 O2 180.0 16 4_665 ?
O2 Fe1 O3 90.88(13) . 13_665 ?
O2 Fe1 O3 89.12(13) 13_665 13_665 ?
O2 Fe1 O3 90.88(13) 16 13_665 ?
O2 Fe1 O3 89.12(13) 4_665 13_665 ?
O2 Fe1 O3 89.12(13) . . ?
O2 Fe1 O3 90.88(13) 13_665 . ?
O2 Fe1 O3 89.12(13) 16 . ?
O2 Fe1 O3 90.88(13) 4_665 . ?
O3 Fe1 O3 180.0 13_665 . ?
C4 O1 Tb1 123.9(3) . . ?
C4 O2 Fe1 132.8(3) . . ?
C3 N1 C3 119.0(5) 12_565 . ?
C3 N1 Tb1 120.5(3) 12_565 . ?
C3 N1 Tb1 120.5(3) . . ?
C2 C1 C2 119.2(7) . 12_565 ?
C2 C1 H1 120.4 . . ?
C2 C1 H1 120.4 12_565 . ?
C3 C2 C1 119.0(5) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
N1 C3 C2 121.9(4) . . ?
N1 C3 C4 114.5(4) . . ?
C2 C3 C4 123.6(4) . . ?
O2 C4 O1 126.5(4) . . ?
O2 C4 C3 117.0(4) . . ?
O1 C4 C3 116.5(4) . . ?
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
Tb1 O1 2.434(3) 3_565 ?
Tb1 O1 2.434(3) 12_565 ?
Tb1 O1 2.434(3) 11 ?
Tb1 O1 2.434(3) 2_665 ?
Tb1 O1 2.434(3) . ?
Tb1 O1 2.434(3) 10_665 ?
Tb1 N1 2.486(5) 2_665 ?
Tb1 N1 2.486(5) 3_565 ?
Tb1 N1 2.486(5) . ?
Fe1 O2 2.090(3) . ?
Fe1 O2 2.090(3) 13_665 ?
Fe1 O2 2.090(3) 16 ?
Fe1 O2 2.090(3) 4_665 ?
Fe1 O3 2.198(4) 13_665 ?
Fe1 O3 2.198(4) . ?
O1 C4 1.262(6) . ?
O2 C4 1.239(5) . ?
N1 C3 1.333(5) 12_565 ?
N1 C3 1.333(5) . ?
C1 C2 1.373(6) . ?
C1 C2 1.373(6) 12_565 ?
C1 H1 0.9300 . ?
C2 C3 1.372(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.500(6) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Tb1 O1 C4 162.3(4) 3_565 . . . ?
O1 Tb1 O1 C4 5.4(3) 12_565 . . . ?
O1 Tb1 O1 C4 -131.3(4) 11 . . . ?
O1 Tb1 O1 C4 81.8(4) 2_665 . . . ?
O1 Tb1 O1 C4 -67.2(3) 10_665 . . . ?
N1 Tb1 O1 C4 112.8(3) 2_665 . . . ?
N1 Tb1 O1 C4 -131.3(4) 3_565 . . . ?
N1 Tb1 O1 C4 5.4(3) . . . . ?
O2 Fe1 O2 C4 15(100) 13_665 . . . ?
O2 Fe1 O2 C4 103.2(5) 16 . . . ?
O2 Fe1 O2 C4 -76.8(5) 4_665 . . . ?
O3 Fe1 O2 C4 12.4(5) 13_665 . . . ?
O3 Fe1 O2 C4 -167.6(5) . . . . ?
O1 Tb1 N1 C3 143.8(3) 3_565 . . 12_565 ?
O1 Tb1 N1 C3 -2.2(2) 12_565 . . 12_565 ?
O1 Tb1 N1 C3 -36.2(3) 11 . . 12_565 ?
O1 Tb1 N1 C3 92.5(3) 2_665 . . 12_565 ?
O1 Tb1 N1 C3 177.8(2) . . . 12_565 ?
O1 Tb1 N1 C3 -87.5(3) 10_665 . . 12_565 ?
N1 Tb1 N1 C3 47.0(2) 2_665 . . 12_565 ?
N1 Tb1 N1 C3 -133.0(2) 3_565 . . 12_565 ?
O1 Tb1 N1 C3 -36.2(3) 3_565 . . . ?
O1 Tb1 N1 C3 177.8(2) 12_565 . . . ?
O1 Tb1 N1 C3 143.8(3) 11 . . . ?
O1 Tb1 N1 C3 -87.5(3) 2_665 . . . ?
O1 Tb1 N1 C3 -2.2(2) . . . . ?
O1 Tb1 N1 C3 92.5(3) 10_665 . . . ?
N1 Tb1 N1 C3 -133.0(2) 2_665 . . . ?
N1 Tb1 N1 C3 47.0(2) 3_565 . . . ?
C2 C1 C2 C3 -0.4(4) 12_565 . . . ?
C3 N1 C3 C2 -0.5(4) 12_565 . . . ?
Tb1 N1 C3 C2 179.5(4) . . . . ?
C3 N1 C3 C4 179.6(5) 12_565 . . . ?
Tb1 N1 C3 C4 -0.4(5) . . . . ?
C1 C2 C3 N1 0.9(8) . . . . ?
C1 C2 C3 C4 -179.2(4) . . . . ?
Fe1 O2 C4 O1 2.1(8) . . . . ?
Fe1 O2 C4 C3 -178.2(3) . . . . ?
Tb1 O1 C4 O2 172.0(4) . . . . ?
Tb1 O1 C4 C3 -7.6(6) . . . . ?
N1 C3 C4 O2 -174.7(4) . . . . ?
C2 C3 C4 O2 5.4(8) . . . . ?
N1 C3 C4 O1 5.0(6) . . . . ?
C2 C3 C4 O1 -174.9(5) . . . . ?
