#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:46:04 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179127 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/89/4308903.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_4308903
loop_
_publ_author_name
'Xiaodan Guo'
'Guangshan Zhu'
'Qianrong Fang'
'Ming Xue'
'Ge Tian'
'Jinyu Sun'
'Xiaotian Li'
'Shilun Qiu'
_publ_section_title
;
Synthesis, Structure and Luminescent Properties of Rare Earth Coordination
Polymers Constructed from Paddle-Wheel Building Blocks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3850
_journal_page_last               3855
_journal_paper_doi               10.1021/ic0500457
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C21 H14 N0 O7 Tb'
_chemical_formula_weight         537.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 107.3250(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.3477(8)
_cell_length_b                   17.1399(8)
_cell_length_c                   18.4904(8)
_cell_measurement_temperature    273(2)
_cell_volume                     7668.8(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'SHELXS-97 (Sheldrick, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.879
_diffrn_measured_fraction_theta_max 0.879
_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  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22753
_diffrn_reflns_theta_full        28.21
_diffrn_reflns_theta_max         28.21
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.865
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.931
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.816
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.308
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         8327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.308
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          0.151
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0622P)²+93.0245P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1917
_refine_ls_wR_factor_ref         0.1951
_reflns_number_gt                7206
_reflns_number_total             8327
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0500457si20050112_103555_1.cif
_cod_data_source_block           Tb(bpdc)1.5(H2O)
_cod_database_code               4308903
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -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
Tb1 Tb 0.497520(8) 0.458942(14) 0.104041(12) 0.03132(6) Uani 1 1 d . . .
O1 O 0.56619(15) 0.5568(2) 0.1376(2) 0.0485(11) Uani 1 1 d . . .
O2 O 0.55676(16) 0.5679(3) 0.0170(3) 0.0556(12) Uani 1 1 d . . .
O3 O 0.45108(14) 0.5737(2) 0.0598(2) 0.0445(10) Uani 1 1 d . . .
O4 O 0.43707(14) 0.6065(3) -0.0607(2) 0.0515(11) Uani 1 1 d . . .
O5 O 0.42744(13) 0.4681(2) 0.1596(2) 0.0413(9) Uani 1 1 d . . .
O6 O 0.44779(15) 0.4250(3) 0.2791(2) 0.0533(11) Uani 1 1 d . . .
O7 O 0.4725(2) 0.3247(3) 0.1161(3) 0.0744(15) Uani 1 1 d . . .
C1 C 0.5792(2) 0.5875(3) 0.0845(4) 0.0473(15) Uani 1 1 d . . .
C2 C 0.6262(2) 0.6434(4) 0.1031(3) 0.0502(16) Uani 1 1 d . . .
C3 C 0.6501(3) 0.6680(5) 0.1773(4) 0.077(2) Uani 1 1 d . . .
H3A H 0.6356 0.6513 0.2153 0.080 Uiso 1 1 calc R . .
C4 C 0.6951(3) 0.7167(5) 0.1947(4) 0.086(2) Uani 1 1 d . . .
H4A H 0.7115 0.7307 0.2450 0.080 Uiso 1 1 calc R . .
C5 C 0.7168(2) 0.7457(4) 0.1401(3) 0.0577(17) Uani 1 1 d . . .
C6 C 0.6910(3) 0.7218(5) 0.0657(4) 0.077(2) Uani 1 1 d . . .
H6A H 0.7046 0.7395 0.0273 0.080 Uiso 1 1 calc R . .
C7 C 0.6464(3) 0.6732(5) 0.0479(4) 0.079(2) Uani 1 1 d . . .
H7A H 0.6294 0.6601 -0.0024 0.080 Uiso 1 1 calc R . .
C8 C 0.42467(19) 0.6068(3) 0.0003(3) 0.0362(12) Uani 1 1 d . . .
C9 C 0.3736(2) 0.6499(3) 0.0010(3) 0.0454(14) Uani 1 1 d . . .
C10 C 0.3491(3) 0.7047(5) -0.0544(4) 0.092(2) Uani 1 1 d . . .
H10A H 0.3650 0.7145 -0.0929 0.080 Uiso 1 1 calc R . .
C11 C 0.3021(3) 0.7449(5) -0.0541(4) 0.077(2) Uani 1 1 d . . .
H11A H 0.2877 0.7825 -0.0909 0.080 Uiso 1 1 calc R . .
C12 C 0.2760(2) 0.7298(4) 0.0003(4) 0.0609(18) Uani 1 1 d . . .
C13 C 0.3013(3) 0.6768(5) 0.0574(4) 0.088(2) Uani 1 1 d . . .
H13A H 0.2856 0.6670 0.0960 0.080 Uiso 1 1 calc R . .
C14 C 0.3493(3) 0.6388(4) 0.0574(4) 0.0726(19) Uani 1 1 d . . .
H14A H 0.3657 0.6046 0.0968 0.080 Uiso 1 1 calc R . .
C15 C 0.41624(17) 0.4309(3) 0.2128(3) 0.0315(11) Uani 1 1 d . . .
C16 C 0.3632(2) 0.3871(3) 0.1954(3) 0.0410(13) Uani 1 1 d . . .
C17 C 0.3222(2) 0.3971(4) 0.1264(3) 0.0558(17) Uani 1 1 d . . .
H17A H 0.3272 0.4335 0.0917 0.080 Uiso 1 1 calc R . .
C18 C 0.2735(2) 0.3530(5) 0.1088(4) 0.065(2) Uani 1 1 d . . .
H18A H 0.2464 0.3607 0.0628 0.080 Uiso 1 1 calc R . .
C19 C 0.2654(2) 0.2983(4) 0.1588(3) 0.0569(17) Uani 1 1 d . . .
C20 C 0.3061(3) 0.2894(5) 0.2289(3) 0.076(2) Uani 1 1 d . . .
H20A H 0.3005 0.2542 0.2641 0.080 Uiso 1 1 calc R . .
C21 C 0.3544(3) 0.3322(4) 0.2464(3) 0.0608(18) Uani 1 1 d . . .
H21A H 0.3814 0.3243 0.2925 0.080 Uiso 1 1 calc 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'
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'
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
O6 Tb1 O2 153.53(17) 2_655 5_665 ?
O6 Tb1 O5 85.77(13) 2_655 . ?
O2 Tb1 O5 97.48(14) 5_665 . ?
O6 Tb1 O3 131.09(15) 2_655 . ?
O2 Tb1 O3 74.46(15) 5_665 . ?
O5 Tb1 O3 73.83(13) . . ?
O6 Tb1 O4 84.77(14) 2_655 5_665 ?
O2 Tb1 O4 81.35(14) 5_665 5_665 ?
O5 Tb1 O4 154.95(14) . 5_665 ?
O3 Tb1 O4 128.79(14) . 5_665 ?
O6 Tb1 O1 74.85(15) 2_655 . ?
O2 Tb1 O1 125.35(16) 5_665 . ?
O5 Tb1 O1 116.08(14) . . ?
O3 Tb1 O1 75.33(13) . . ?
O4 Tb1 O1 83.58(15) 5_665 . ?
O6 Tb1 O7 76.72(17) 2_655 . ?
O2 Tb1 O7 78.54(17) 5_665 . ?
O5 Tb1 O7 76.42(16) . . ?
O3 Tb1 O7 136.30(15) . . ?
O4 Tb1 O7 78.85(17) 5_665 . ?
O1 Tb1 O7 147.71(15) . . ?
C1 O1 Tb1 116.2(3) . . ?
C1 O2 Tb1 170.4(4) . 5_665 ?
C8 O3 Tb1 141.7(4) . . ?
C8 O4 Tb1 134.7(3) . 5_665 ?
C15 O5 Tb1 133.6(3) . . ?
C15 O6 Tb1 160.4(4) . 2_655 ?
O1 C1 O2 121.7(5) . . ?
O1 C1 C2 118.3(5) . . ?
O2 C1 C2 119.8(6) . . ?
C7 C2 C3 118.2(6) . . ?
C7 C2 C1 121.3(5) . . ?
C3 C2 C1 120.5(6) . . ?
C4 C3 C2 120.3(6) . . ?
C3 C4 C5 122.1(6) . . ?
C4 C5 C6 116.3(6) . . ?
C4 C5 C19 122.2(6) . 3 ?
C6 C5 C19 121.4(6) . 3 ?
C7 C6 C5 121.9(6) . . ?
C6 C7 C2 121.0(6) . . ?
O3 C8 O4 125.4(5) . . ?
O3 C8 C9 117.3(5) . . ?
O4 C8 C9 117.2(4) . . ?
C14 C9 C10 116.7(5) . . ?
C14 C9 C8 121.5(5) . . ?
C10 C9 C8 121.7(5) . . ?
C11 C10 C9 122.0(7) . . ?
C10 C11 C12 120.8(7) . . ?
C11 C12 C13 117.4(6) . . ?
C11 C12 C12 121.5(7) . 7_565 ?
C13 C12 C12 121.0(8) . 7_565 ?
C14 C13 C12 120.9(7) . . ?
C9 C14 C13 121.9(6) . . ?
O6 C15 O5 125.0(4) . . ?
O6 C15 C16 116.3(5) . . ?
O5 C15 C16 118.6(4) . . ?
C17 C16 C21 118.3(5) . . ?
C17 C16 C15 121.0(5) . . ?
C21 C16 C15 120.6(4) . . ?
C16 C17 C18 120.7(6) . . ?
C19 C18 C17 120.7(5) . . ?
C18 C19 C20 118.6(6) . . ?
C18 C19 C5 122.6(5) . 3_445 ?
C20 C19 C5 118.8(6) . 3_445 ?
C21 C20 C19 121.1(6) . . ?
C20 C21 C16 120.6(5) . . ?
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 O6 2.269(4) 2_655 ?
Tb1 O2 2.299(4) 5_665 ?
Tb1 O5 2.307(4) . ?
Tb1 O3 2.313(4) . ?
Tb1 O4 2.332(4) 5_665 ?
Tb1 O1 2.363(4) . ?
Tb1 O7 2.415(5) . ?
O1 C1 1.242(8) . ?
O2 C1 1.253(7) . ?
O2 Tb1 2.298(4) 5_665 ?
O3 C8 1.242(6) . ?
O4 C8 1.258(7) . ?
O4 Tb1 2.333(4) 5_665 ?
O5 C15 1.274(6) . ?
O6 C15 1.251(6) . ?
O6 Tb1 2.269(4) 2_655 ?
C1 C2 1.487(8) . ?
C2 C7 1.368(10) . ?
C2 C3 1.390(8) . ?
C3 C4 1.372(10) . ?
C4 C5 1.378(10) . ?
C5 C6 1.397(9) . ?
C5 C19 1.483(8) 3 ?
C6 C7 1.363(10) . ?
C8 C9 1.492(7) . ?
C9 C14 1.374(9) . ?
C9 C10 1.393(9) . ?
C10 C11 1.378(9) . ?
C11 C12 1.383(10) . ?
C12 C13 1.395(10) . ?
C12 C12 1.487(12) 7_565 ?
C13 C14 1.381(9) . ?
C15 C16 1.488(7) . ?
C16 C17 1.397(7) . ?
C16 C21 1.396(9) . ?
C17 C18 1.400(8) . ?
C18 C19 1.375(10) . ?
C19 C20 1.404(8) . ?
C19 C5 1.483(8) 3_445 ?
C20 C21 1.380(9) . ?
