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#$Date: 2016-03-22 11:32:17 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178903 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/32/4113226.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_4113226
loop_
_publ_author_name
'Bin Zhao'
'Xiao-Yan Chen'
'Peng Cheng'
'Dai-Zheng Liao'
'Shi-Ping Yan'
'Zong-Hui Jiang'
_publ_section_title
;
 Coordination Polymers Containing 1D Channels as Selective Luminescent
 Probes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15394
_journal_page_last               15395
_journal_paper_doi               10.1021/ja047141b
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C21 H21.5 Mn1.5 N3 O18.25 Tb'
_chemical_formula_weight         849.24
_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                   15.351(4)
_cell_length_b                   15.351(4)
_cell_length_c                   15.812(8)
_cell_measurement_reflns_used    710
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      23.19
_cell_measurement_theta_min      2.58
_cell_volume                     3227(2)
_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      273(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_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  0.2016
_diffrn_reflns_av_sigmaI/netI    0.0729
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11657
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    2.831
_exptl_absorpt_correction_T_max  0.6014
_exptl_absorpt_correction_T_min  0.4839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_meas      0
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.985
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         962
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0575P)²+13.7248P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1162
_reflns_number_gt                604
_reflns_number_total             962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja047141bsi20040515_115653.cif
_cod_data_source_block           020609c
_cod_original_cell_volume        3227.1(19)
_cod_database_code               4113226
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
Tb1 Tb 0.6667 0.3333 0.2500 0.02038(1) Uani 1 6 d S
Mn1 Mn 0.5000 0.5000 0.0000 0.02068(5) Uani 1 4 d S
N1 N 0.47923(5) 0.23961(2) 0.2500 0.02366(15) Uani 1 2 d S
O1 O 0.44922(3) 0.38422(3) 0.09331(3) 0.04335(16) Uani 1 1 d .
O2 O 0.58720(3) 0.38758(3) 0.14458(3) 0.03501(14) Uani 1 1 d .
O3 O 0.65349(4) 0.50911(4) 0.0000 0.0339(2) Uani 1 2 d S
O4 O 0.79131(16) 0.72648(15) 0.0000 0.2550(13) Uani 1 2 d S
C1 C 0.49385(4) 0.35265(4) 0.13999(4) 0.02755(19) Uani 1 1 d .
C2 C 0.42750(4) 0.26544(4) 0.19739(4) 0.02898(19) Uani 1 1 d .
C3 C 0.32513(5) 0.21513(5) 0.19464(5) 0.0439(3) Uani 1 1 d .
H3A H 0.2913 0.2335 0.1562 0.053 Uiso 1 1 calc R
C4 C 0.27244(7) 0.13622(3) 0.2500 0.0531(3) Uani 1 2 d S
H4 H 0.2025 0.1012 0.2500 0.064 Uiso 1 2 calc SR
O5 O 0.00000(7) 0.00000(3) 0.2500 0.10151(6) Uani 0.50 12 d SPRU
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'
Mn Mn 0.3368 0.7283 '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
O2 Tb1 O2 128.79(2) 11_655 2_655
O2 Tb1 O2 78.61(3) 11_655 12
O2 Tb1 O2 86.70(4) 2_655 12
O2 Tb1 O2 86.70(4) 11_655 3_665
O2 Tb1 O2 78.61(3) 2_655 3_665
O2 Tb1 O2 145.688(18) 12 3_665
O2 Tb1 O2 78.61(3) 11_655 10_665
O2 Tb1 O2 145.688(18) 2_655 10_665
O2 Tb1 O2 78.61(3) 12 10_665
O2 Tb1 O2 128.79(2) 3_665 10_665
O2 Tb1 O2 145.687(18) 11_655 .
O2 Tb1 O2 78.61(3) 2_655 .
O2 Tb1 O2 128.79(2) 12 .
O2 Tb1 O2 78.61(3) 3_665 .
O2 Tb1 O2 86.70(4) 10_665 .
O2 Tb1 N1 64.394(11) 11_655 2_655
O2 Tb1 N1 64.394(10) 2_655 2_655
O2 Tb1 N1 72.844(9) 12 2_655
O2 Tb1 N1 72.844(9) 3_665 2_655
O2 Tb1 N1 136.648(19) 10_665 2_655
O2 Tb1 N1 136.648(19) . 2_655
O2 Tb1 N1 72.844(9) 11_655 3_665
O2 Tb1 N1 136.648(19) 2_655 3_665
O2 Tb1 N1 136.648(19) 12 3_665
O2 Tb1 N1 64.394(10) 3_665 3_665
O2 Tb1 N1 64.394(10) 10_665 3_665
O2 Tb1 N1 72.843(9) . 3_665
N1 Tb1 N1 120.0 2_655 3_665
O2 Tb1 N1 136.648(19) 11_655 .
O2 Tb1 N1 72.844(9) 2_655 .
O2 Tb1 N1 64.394(11) 12 .
O2 Tb1 N1 136.648(19) 3_665 .
O2 Tb1 N1 72.844(9) 10_665 .
O2 Tb1 N1 64.395(10) . .
N1 Tb1 N1 120.0 2_655 .
N1 Tb1 N1 120.0 3_665 .
O1 Mn1 O1 87.43(4) . 16
O1 Mn1 O1 92.57(4) . 4_665
O1 Mn1 O1 180.00(3) 16 4_665
O1 Mn1 O1 180.000(18) . 13_665
O1 Mn1 O1 92.57(4) 16 13_665
O1 Mn1 O1 87.43(4) 4_665 13_665
O1 Mn1 O3 89.261(17) . .
O1 Mn1 O3 89.261(17) 16 .
O1 Mn1 O3 90.739(17) 4_665 .
O1 Mn1 O3 90.739(17) 13_665 .
O1 Mn1 O3 90.740(17) . 13_665
O1 Mn1 O3 90.740(17) 16 13_665
O1 Mn1 O3 89.260(17) 4_665 13_665
O1 Mn1 O3 89.260(17) 13_665 13_665
O3 Mn1 O3 180.0 . 13_665
C2 N1 C2 118.22(6) 12 .
C2 N1 Tb1 120.89(3) 12 .
C2 N1 Tb1 120.89(3) . .
C1 O1 Mn1 133.16(4) . .
C1 O2 Tb1 123.44(4) . .
O2 C1 O1 126.48(5) . .
O2 C1 C2 117.55(6) . .
O1 C1 C2 115.95(5) . .
N1 C2 C3 122.60(6) . .
N1 C2 C1 113.45(5) . .
C3 C2 C1 123.92(7) . .
C2 C3 C4 118.74(7) . .
C2 C3 H3A 120.6 . .
C4 C3 H3A 120.6 . .
C3 C4 C3 119.06(9) 12 .
C3 C4 H4 120.5 12 .
C3 C4 H4 120.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O2 2.4446(8) 11_655
Tb1 O2 2.4446(8) 2_655
Tb1 O2 2.4446(8) 12
Tb1 O2 2.4446(8) 3_665
Tb1 O2 2.4446(8) 10_665
Tb1 O2 2.4446(8) .
Tb1 N1 2.4919(9) 2_655
Tb1 N1 2.4919(9) 3_665
Tb1 N1 2.4919(9) .
Mn1 O1 2.1350(7) .
Mn1 O1 2.1351(7) 16
Mn1 O1 2.1351(7) 4_665
Mn1 O1 2.1351(7) 13_665
Mn1 O3 2.2895(9) .
Mn1 O3 2.2895(9) 13_665
N1 C2 1.3396(8) 12
N1 C2 1.3396(8) .
O1 C1 1.2574(9) .
O2 C1 1.2562(8) .
C1 C2 1.5133(8) .
C2 C3 1.3617(9) .
C3 C4 1.3814(9) .
C3 H3A 0.9300 .
C4 C3 1.3814(9) 12
C4 H4 0.9300 .
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_4
O2 Tb1 N1 C2 -37.03(4) 11_655 12
O2 Tb1 N1 C2 91.88(5) 2_655 12
O2 Tb1 N1 C2 -2.78(4) 12 12
O2 Tb1 N1 C2 142.97(4) 3_665 12
O2 Tb1 N1 C2 -88.12(5) 10_665 12
O2 Tb1 N1 C2 177.22(4) . 12
N1 Tb1 N1 C2 46.35(4) 2_655 12
N1 Tb1 N1 C2 -133.65(4) 3_665 12
O2 Tb1 N1 C2 142.98(4) 11_655 .
O2 Tb1 N1 C2 -88.12(5) 2_655 .
O2 Tb1 N1 C2 177.22(4) 12 .
O2 Tb1 N1 C2 -37.02(4) 3_665 .
O2 Tb1 N1 C2 91.88(5) 10_665 .
O2 Tb1 N1 C2 -2.78(4) . .
N1 Tb1 N1 C2 -133.65(4) 2_655 .
N1 Tb1 N1 C2 46.35(4) 3_665 .
O1 Mn1 O1 C1 102.51(5) 16 .
O1 Mn1 O1 C1 -77.49(5) 4_665 .
O1 Mn1 O1 C1 -174(25) 13_665 .
O3 Mn1 O1 C1 13.22(6) . .
O3 Mn1 O1 C1 -166.78(6) 13_665 .
O2 Tb1 O2 C1 -131.88(5) 11_655 .
O2 Tb1 O2 C1 81.14(5) 2_655 .
O2 Tb1 O2 C1 4.86(4) 12 .
O2 Tb1 O2 C1 161.65(5) 3_665 .
O2 Tb1 O2 C1 -67.68(5) 10_665 .
N1 Tb1 O2 C1 112.32(5) 2_655 .
N1 Tb1 O2 C1 -131.88(5) 3_665 .
N1 Tb1 O2 C1 4.86(4) . .
Tb1 O2 C1 O1 172.21(5) . .
Tb1 O2 C1 C2 -6.23(8) . .
Mn1 O1 C1 O2 2.80(10) . .
Mn1 O1 C1 C2 -178.74(4) . .
C2 N1 C2 C3 -1.01(5) 12 .
Tb1 N1 C2 C3 178.98(5) . .
C2 N1 C2 C1 -178.91(6) 12 .
Tb1 N1 C2 C1 1.09(6) . .
O2 C1 C2 N1 3.18(8) . .
O1 C1 C2 N1 -175.42(5) . .
O2 C1 C2 C3 -174.68(7) . .
O1 C1 C2 C3 6.72(10) . .
N1 C2 C3 C4 1.98(10) . .
C1 C2 C3 C4 179.65(6) . .
C2 C3 C4 C3 -0.95(5) . 12
