#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:05:22 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179230 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/50/4315012.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_4315012
loop_
_publ_author_name
'You-Wen Lin'
'Bo-Ren Jian'
'Sin-Chiang Huang'
'Chin-Her Huang'
'Kuei-Fang Hsu'
_publ_section_title
;
 Synthesis and Characterization of Three Ytterbium Coordination Polymers
 Featuring Various Cationic Species and a Luminescence Study of a Terbium
 Analogue With Open Channels
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2316
_journal_page_last               2324
_journal_paper_doi               10.1021/ic9021992
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         '[NH3(CH2)2NH3]0.5[Yb(C12H8OC2O4)(H2O)]'
_chemical_formula_sum            'C29 H23 N O11 Yb'
_chemical_formula_weight         734.52
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.9450(10)
_cell_angle_beta                 76.2590(10)
_cell_angle_gamma                88.2540(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5795(2)
_cell_length_b                   10.4344(2)
_cell_length_c                   14.6343(3)
_cell_measurement_reflns_used    8362
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.38
_cell_measurement_theta_min      2.86
_cell_volume                     1349.48(5)
_computing_cell_refinement       'Bruker SMART APEX II'
_computing_data_collection       'Bruker SMART APEX II'
_computing_data_reduction        'Bruker SMART APEX II'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0578
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29197
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    3.531
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.53740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.118
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6522
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0392P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0572
_reflns_number_gt                5904
_reflns_number_total             6522
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9021992_si_002_1.cif
_cod_data_source_block           compound1
_cod_database_code               4315012
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Yb1 Yb 0.719819(11) 0.632388(10) 0.507022(7) 0.01938(4) Uani 1 1 d . . .
O1 O 0.8288(2) 0.6596(2) 0.61527(14) 0.0328(5) Uani 1 1 d . . .
O2 O 0.7818(2) 0.8023(2) 0.70334(16) 0.0375(5) Uani 1 1 d . . .
O3 O 0.8537(3) 0.2639(2) 1.03673(16) 0.0443(6) Uani 1 1 d . . .
O4 O 0.6493(2) 0.2296(2) 1.48919(16) 0.0317(4) Uani 1 1 d . . .
O5 O 0.4371(2) 0.2192(2) 1.45486(15) 0.0326(5) Uani 1 1 d . . .
O6 O 0.6400(2) 0.6080(2) 0.38624(14) 0.0339(5) Uani 1 1 d . . .
O7 O 0.4513(2) 0.5033(2) 0.37533(15) 0.0364(5) Uani 1 1 d . . .
O8 O 0.6158(2) 0.8885(2) -0.06101(14) 0.0371(5) Uani 1 1 d . . .
O9 O 1.18226(19) 1.15787(19) -0.38705(14) 0.0266(4) Uani 1 1 d . . .
O10 O 1.03690(19) 1.32436(19) -0.41186(14) 0.0283(4) Uani 1 1 d . . .
O11 O 0.8091(2) 0.4244(2) 0.50997(17) 0.0384(5) Uani 1 1 d . . .
C1 C 0.8080(3) 0.6878(3) 0.6964(2) 0.0273(6) Uani 1 1 d . . .
C2 C 0.8190(3) 0.5761(3) 0.7867(2) 0.0269(6) Uani 1 1 d . . .
C3 C 0.7590(3) 0.5878(3) 0.8804(2) 0.0292(6) Uani 1 1 d . . .
H3B H 0.7123 0.6656 0.8857 0.050 Uiso 1 1 calc . . .
C4 C 0.8897(3) 0.4595(3) 0.7804(2) 0.0328(6) Uani 1 1 d . . .
H4A H 0.9293 0.4497 0.7186 0.050 Uiso 1 1 calc . . .
C5 C 0.7679(3) 0.4862(3) 0.9651(2) 0.0324(6) Uani 1 1 d . . .
H5A H 0.7266 0.4948 1.0271 0.050 Uiso 1 1 calc . . .
C6 C 0.9017(4) 0.3587(3) 0.8645(2) 0.0367(7) Uani 1 1 d . . .
H6A H 0.9516 0.2823 0.8595 0.050 Uiso 1 1 calc . . .
C7 C 0.8390(3) 0.3715(3) 0.9570(2) 0.0306(6) Uani 1 1 d . . .
C8 C 0.7807(3) 0.2632(3) 1.1322(2) 0.0327(7) Uani 1 1 d . . .
C9 C 0.8494(3) 0.3139(4) 1.1860(2) 0.0399(7) Uani 1 1 d . . .
H9A H 0.9405 0.3561 1.1575 0.050 Uiso 1 1 calc . . .
C10 C 0.6446(4) 0.2018(4) 1.1719(2) 0.0443(8) Uani 1 1 d . . .
H10A H 0.5995 0.1667 1.1346 0.050 Uiso 1 1 calc . . .
C11 C 0.7829(3) 0.3023(3) 1.2831(2) 0.0367(7) Uani 1 1 d . . .
H11A H 0.8305 0.3349 1.3205 0.050 Uiso 1 1 calc . . .
C12 C 0.5771(3) 0.1935(4) 1.2680(2) 0.0413(8) Uani 1 1 d . . .
H12A H 0.4843 0.1549 1.2949 0.050 Uiso 1 1 calc . . .
C13 C 0.6454(3) 0.2421(3) 1.3255(2) 0.0281(6) Uani 1 1 d . . .
C14 C 0.5735(3) 0.2302(3) 1.4309(2) 0.0250(5) Uani 1 1 d . . .
C15 C 0.5564(3) 0.5866(3) 0.33866(19) 0.0231(5) Uani 1 1 d . . .
C16 C 0.5824(3) 0.6633(3) 0.23141(19) 0.0227(5) Uani 1 1 d . . .
C17 C 0.6770(3) 0.7773(3) 0.1899(2) 0.0289(6) Uani 1 1 d . . .
H17A H 0.7288 0.8020 0.2286 0.050 Uiso 1 1 calc . . .
C18 C 0.5088(3) 0.6264(3) 0.1720(2) 0.0285(6) Uani 1 1 d . . .
H18A H 0.4462 0.5506 0.1988 0.050 Uiso 1 1 calc . . .
C19 C 0.6941(3) 0.8539(3) 0.0912(2) 0.0324(7) Uani 1 1 d . . .
H19A H 0.7559 0.9303 0.0638 0.050 Uiso 1 1 calc . . .
C20 C 0.5272(3) 0.7009(3) 0.0737(2) 0.0298(6) Uani 1 1 d . . .
H20A H 0.4785 0.6745 0.0341 0.050 Uiso 1 1 calc . . .
C21 C 0.6180(3) 0.8147(3) 0.03449(19) 0.0262(6) Uani 1 1 d . . .
C22 C 0.7322(3) 0.9661(3) -0.12788(19) 0.0266(6) Uani 1 1 d . . .
C23 C 0.8731(3) 0.9313(3) -0.1328(2) 0.0307(6) Uani 1 1 d . . .
H23A H 0.8962 0.8573 -0.0848 0.050 Uiso 1 1 calc . . .
C24 C 0.6964(3) 1.0790(3) -0.1962(2) 0.0314(6) Uani 1 1 d . . .
H24A H 0.6008 1.1016 -0.1913 0.050 Uiso 1 1 calc . . .
C25 C 0.9797(3) 1.0087(3) -0.2107(2) 0.0275(6) Uani 1 1 d . . .
H25A H 1.0748 0.9844 -0.2167 0.050 Uiso 1 1 calc . . .
C26 C 0.8034(3) 1.1574(3) -0.2716(2) 0.0298(6) Uani 1 1 d . . .
H26A H 0.7803 1.2343 -0.3172 0.050 Uiso 1 1 calc . . .
C27 C 0.9457(3) 1.1223(3) -0.27986(19) 0.0237(5) Uani 1 1 d . . .
C28 C 1.0607(3) 1.2053(3) -0.36344(19) 0.0220(5) Uani 1 1 d . . .
C29 C 0.9468(3) 0.0531(3) 1.4836(2) 0.0321(6) Uani 1 1 d . . .
N1 N 0.7982(3) -0.0073(2) 1.52482(19) 0.0314(5) Uani 1 1 d . . .
H1A H 0.7729 -0.0406 1.4817 0.050 Uiso 1 1 calc . . .
H1B H 0.7381 0.0558 1.5363 0.050 Uiso 1 1 calc . . .
H1C H 0.7944 -0.0732 1.5813 0.050 Uiso 1 1 calc . . .
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'
Yb Yb -0.3850 5.5486 '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 Yb1 O1 172.32(7) . . ?
O6 Yb1 O7 94.37(8) . 2_666 ?
O1 Yb1 O7 92.10(8) . 2_666 ?
O6 Yb1 O5 97.35(8) . 2_667 ?
O1 Yb1 O5 87.97(8) . 2_667 ?
O7 Yb1 O5 78.72(8) 2_666 2_667 ?
O6 Yb1 O11 82.10(8) . . ?
O1 Yb1 O11 95.10(8) . . ?
O7 Yb1 O11 79.04(8) 2_666 . ?
O5 Yb1 O11 157.64(8) 2_667 . ?
O6 Yb1 O10 93.62(7) . 2_775 ?
O1 Yb1 O10 78.72(7) . 2_775 ?
O7 Yb1 O10 150.70(8) 2_666 2_775 ?
O5 Yb1 O10 127.99(7) 2_667 2_775 ?
O11 Yb1 O10 74.21(7) . 2_775 ?
O6 Yb1 O9 82.97(7) . 2_775 ?
O1 Yb1 O9 92.93(7) . 2_775 ?
O7 Yb1 O9 154.64(8) 2_666 2_775 ?
O5 Yb1 O9 76.64(7) 2_667 2_775 ?
O11 Yb1 O9 125.15(7) . 2_775 ?
O10 Yb1 O9 54.51(6) 2_775 2_775 ?
O6 Yb1 C28 86.60(8) . 2_775 ?
O1 Yb1 C28 86.80(8) . 2_775 ?
O7 Yb1 C28 177.99(8) 2_666 2_775 ?
O5 Yb1 C28 102.92(8) 2_667 2_775 ?
O11 Yb1 C28 99.37(8) . 2_775 ?
O10 Yb1 C28 27.35(7) 2_775 2_775 ?
O9 Yb1 C28 27.24(7) 2_775 2_775 ?
O6 Yb1 C14 87.30(8) . 2_667 ?
O1 Yb1 C14 99.25(8) . 2_667 ?
O7 Yb1 C14 64.43(8) 2_666 2_667 ?
O5 Yb1 C14 18.09(7) 2_667 2_667 ?
O11 Yb1 C14 141.00(7) . 2_667 ?
O10 Yb1 C14 144.17(6) 2_775 2_667 ?
O9 Yb1 C14 90.22(6) 2_775 2_667 ?
C28 Yb1 C14 117.41(7) 2_775 2_667 ?
C1 O1 Yb1 143.11(19) . . ?
C7 O3 C8 118.7(2) . . ?
C14 O5 Yb1 128.88(18) . 2_667 ?
C15 O6 Yb1 160.94(19) . . ?
C15 O7 Yb1 157.60(19) . 2_666 ?
C21 O8 C22 123.4(2) . . ?
C28 O9 Yb1 92.89(15) . 2_775 ?
C28 O10 Yb1 92.84(15) . 2_775 ?
O2 C1 O1 123.8(3) . . ?
O2 C1 C2 118.9(3) . . ?
O1 C1 C2 117.2(3) . . ?
C3 C2 C4 118.5(3) . . ?
C3 C2 C1 119.9(3) . . ?
C4 C2 C1 121.5(3) . . ?
C5 C3 C2 121.2(3) . . ?
C5 C3 H3B 119.4 . . ?
C2 C3 H3B 119.4 . . ?
C6 C4 C2 120.8(3) . . ?
C6 C4 H4A 119.6 . . ?
C2 C4 H4A 119.6 . . ?
C7 C5 C3 119.3(3) . . ?
C7 C5 H5A 120.4 . . ?
C3 C5 H5A 120.4 . . ?
C4 C6 C7 119.7(3) . . ?
C4 C6 H6A 120.2 . . ?
C7 C6 H6A 120.2 . . ?
O3 C7 C5 124.0(3) . . ?
O3 C7 C6 115.4(3) . . ?
C5 C7 C6 120.6(3) . . ?
C9 C8 C10 121.6(3) . . ?
C9 C8 O3 119.4(3) . . ?
C10 C8 O3 118.8(3) . . ?
C8 C9 C11 119.6(3) . . ?
C8 C9 H9A 120.2 . . ?
C11 C9 H9A 120.2 . . ?
C12 C10 C8 118.6(3) . . ?
C12 C10 H10A 120.7 . . ?
C8 C10 H10A 120.7 . . ?
C9 C11 C13 120.5(3) . . ?
C9 C11 H11A 119.8 . . ?
C13 C11 H11A 119.8 . . ?
C10 C12 C13 121.1(3) . . ?
C10 C12 H12A 119.4 . . ?
C13 C12 H12A 119.4 . . ?
C12 C13 C11 118.6(3) . . ?
C12 C13 C14 121.3(2) . . ?
C11 C13 C14 120.2(3) . . ?
O4 C14 O5 124.2(3) . . ?
O4 C14 C13 119.0(2) . . ?
O5 C14 C13 116.7(2) . . ?
O4 C14 Yb1 108.88(18) . 2_667 ?
O5 C14 Yb1 33.03(13) . 2_667 ?
C13 C14 Yb1 123.14(17) . 2_667 ?
O6 C15 O7 124.0(2) . . ?
O6 C15 C16 118.7(2) . . ?
O7 C15 C16 117.4(2) . . ?
C18 C16 C17 118.9(2) . . ?
C18 C16 C15 120.5(2) . . ?
C17 C16 C15 120.5(2) . . ?
C19 C17 C16 120.4(3) . . ?
C19 C17 H17A 119.8 . . ?
C16 C17 H17A 119.8 . . ?
C16 C18 C20 120.8(2) . . ?
C16 C18 H18A 119.6 . . ?
C20 C18 H18A 119.6 . . ?
C21 C19 C17 119.0(2) . . ?
C21 C19 H19A 120.5 . . ?
C17 C19 H19A 120.5 . . ?
C21 C20 C18 119.7(2) . . ?
C21 C20 H20A 120.2 . . ?
C18 C20 H20A 120.2 . . ?
O8 C21 C20 114.3(2) . . ?
O8 C21 C19 124.3(3) . . ?
C20 C21 C19 121.2(2) . . ?
C23 C22 O8 124.0(3) . . ?
C23 C22 C24 121.5(2) . . ?
O8 C22 C24 114.4(2) . . ?
C22 C23 C25 118.6(3) . . ?
C22 C23 H23A 120.7 . . ?
C25 C23 H23A 120.7 . . ?
C26 C24 C22 119.4(3) . . ?
C26 C24 H24A 120.3 . . ?
C22 C24 H24A 120.3 . . ?
C27 C25 C23 120.6(3) . . ?
C27 C25 H25A 119.7 . . ?
C23 C25 H25A 119.7 . . ?
C24 C26 C27 120.3(3) . . ?
C24 C26 H26A 119.9 . . ?
C27 C26 H26A 119.9 . . ?
C26 C27 C25 119.6(2) . . ?
C26 C27 C28 120.0(2) . . ?
C25 C27 C28 120.4(2) . . ?
O9 C28 O10 119.4(2) . . ?
O9 C28 C27 120.5(2) . . ?
O10 C28 C27 120.0(2) . . ?
O9 C28 Yb1 59.86(13) . 2_775 ?
O10 C28 Yb1 59.82(13) . 2_775 ?
C27 C28 Yb1 175.19(19) . 2_775 ?
N1 C29 C29 109.4(3) . 2_758 ?
C29 N1 H1A 109.5 . . ?
C29 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C29 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
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
Yb1 O6 2.1696(19) . ?
Yb1 O1 2.1819(19) . ?
Yb1 O7 2.2239(18) 2_666 ?
Yb1 O5 2.228(2) 2_667 ?
Yb1 O11 2.300(2) . ?
Yb1 O10 2.3889(18) 2_775 ?
Yb1 O9 2.3902(18) 2_775 ?
Yb1 C28 2.760(2) 2_775 ?
Yb1 C14 3.182(3) 2_667 ?
O1 C1 1.280(3) . ?
O2 C1 1.243(4) . ?
O3 C7 1.378(4) . ?
O3 C8 1.403(3) . ?
O4 C14 1.242(3) . ?
O5 C14 1.269(3) . ?
O5 Yb1 2.228(2) 2_667 ?
O6 C15 1.244(3) . ?
O7 C15 1.251(3) . ?
O7 Yb1 2.2239(18) 2_666 ?
O8 C21 1.376(3) . ?
O8 C22 1.379(3) . ?
O9 C28 1.265(3) . ?
O9 Yb1 2.3902(18) 2_775 ?
O10 C28 1.270(3) . ?
O10 Yb1 2.3889(18) 2_775 ?
C1 C2 1.489(4) . ?
C2 C3 1.396(4) . ?
C2 C4 1.392(4) . ?
C3 C5 1.378(4) . ?
C3 H3B 0.9300 . ?
C4 C6 1.376(4) . ?
C4 H4A 0.9300 . ?
C5 C7 1.383(4) . ?
C5 H5A 0.9300 . ?
C6 C7 1.390(4) . ?
C6 H6A 0.9300 . ?
C8 C9 1.364(5) . ?
C8 C10 1.381(4) . ?
C9 C11 1.381(4) . ?
C9 H9A 0.9300 . ?
C10 C12 1.379(5) . ?
C10 H10A 0.9300 . ?
C11 C13 1.391(4) . ?
C11 H11A 0.9300 . ?
C12 C13 1.392(4) . ?
C12 H12A 0.9300 . ?
C13 C14 1.501(4) . ?
C14 Yb1 3.182(3) 2_667 ?
C15 C16 1.488(3) . ?
C16 C18 1.384(4) . ?
C16 C17 1.401(4) . ?
C17 C19 1.390(4) . ?
C17 H17A 0.9300 . ?
C18 C20 1.378(4) . ?
C18 H18A 0.9300 . ?
C19 C21 1.379(4) . ?
C19 H19A 0.9300 . ?
C20 C21 1.378(4) . ?
C20 H20A 0.9300 . ?
C22 C23 1.378(4) . ?
C22 C24 1.384(4) . ?
C23 C25 1.386(4) . ?
C23 H23A 0.9300 . ?
C24 C26 1.375(4) . ?
C24 H24A 0.9300 . ?
C25 C27 1.387(4) . ?
C25 H25A 0.9300 . ?
C26 C27 1.387(4) . ?
C26 H26A 0.9300 . ?
C27 C28 1.490(3) . ?
C28 Yb1 2.760(2) 2_775 ?
C29 N1 1.482(4) . ?
C29 C29 1.527(6) 2_758 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
