#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:16:14 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180497 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/66/7216680.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_7216680
loop_
_publ_author_name
'Zhao, Tingting'
'Zhang, Lirong'
'Wang, Dongmei'
'Li, Guanghua'
'Huo, Qisheng'
'Liu, Yunling'
_publ_section_title
;
 Rational design and synthesis of a series of 3D lanthanide metal--organic
 frameworks with different structures driven by reaction conditions
;
_journal_issue                   44
_journal_name_full               CrystEngComm
_journal_page_first              10181
_journal_paper_doi               10.1039/C4CE00858H
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C16 H14 K2 La2 N4 O21 S2'
_chemical_formula_sum            'C16 H14 K2 La2 N4 O21 S2'
_chemical_formula_weight         1018.45
_chemical_melting_point          ?
_chemical_name_systematic
; 
 ? 
;
_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                102.7690(10)
_cell_angle_beta                 109.2740(10)
_cell_angle_gamma                111.5200(10)
_cell_formula_units_Z            1
_cell_length_a                   8.2691(6)
_cell_length_b                   10.3254(7)
_cell_length_c                   10.9614(12)
_cell_measurement_reflns_used    2667
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.14
_cell_volume                     756.93(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0138
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3887
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    3.292
_exptl_absorpt_correction_T_max  0.6147
_exptl_absorpt_correction_T_min  0.4738
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.234
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             490
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         2667
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0347P)²+0.7603P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0637
_reflns_number_gt                2484
_reflns_number_total             2667
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce00858h2.cif
_cod_data_source_block           compound9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7216672--7216683.cif.

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      P-1
_cod_database_code               7216680
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
La1 La 0.32712(3) 1.11038(2) 1.06812(2) 0.01749(9) Uani 1 1 d .
K1 K 0.35519(15) 1.41867(11) 0.81638(11) 0.0343(2) Uani 1 1 d D
S1 S 0.81260(17) 1.41475(15) 0.73250(14) 0.0368(3) Uani 1 1 d .
O1 O 0.6493(5) 1.1351(3) 1.0073(3) 0.0328(7) Uani 1 1 d .
O2 O 0.5415(4) 1.2981(3) 0.9921(3) 0.0299(7) Uani 1 1 d .
O3 O 0.9617(4) 1.1090(3) 0.9620(3) 0.0273(6) Uani 1 1 d .
O4 O 1.2222(4) 1.3097(3) 1.0014(3) 0.0274(6) Uani 1 1 d .
O5 O 0.5185(4) 1.3698(3) 1.2828(3) 0.0328(7) Uani 1 1 d .
O6 O 0.2411(4) 1.2040(3) 1.2619(3) 0.0326(7) Uani 1 1 d .
O7 O 0.5322(5) 1.0873(4) 1.2681(3) 0.0415(8) Uani 1 1 d .
O8 O 0.7377(5) 1.0282(4) 1.3971(4) 0.0445(9) Uani 1 1 d .
O9 O 0.1397(5) 0.9886(4) 0.8046(3) 0.0359(8) Uani 1 1 d D
N1 N 0.6715(5) 1.3558(4) 0.8035(4) 0.0288(8) Uani 1 1 d .
N2 N 0.9735(5) 1.3650(4) 0.8047(4) 0.0308(8) Uani 1 1 d .
C1 C 0.7431(6) 1.2922(4) 0.8847(4) 0.0213(8) Uani 1 1 d .
C2 C 0.9169(6) 1.2964(4) 0.8835(4) 0.0212(8) Uani 1 1 d .
C3 C 0.6397(5) 1.2373(4) 0.9674(4) 0.0209(8) Uani 1 1 d .
C4 C 1.0422(6) 1.2351(4) 0.9564(4) 0.0215(8) Uani 1 1 d .
C5 C 0.4236(6) 1.4331(5) 1.4617(4) 0.0277(9) Uani 1 1 d .
H5 H 0.3293 1.4005 1.4924 0.080 Uiso 1 1 calc .
C6 C 0.3942(6) 1.3312(5) 1.3279(4) 0.0260(9) Uani 1 1 d .
C7 C 0.4801(6) 1.0239(5) 1.4495(5) 0.0298(10) Uani 1 1 d .
H7 H 0.3754 1.0438 1.4273 0.080 Uiso 1 1 calc .
C8 C 0.5924(6) 1.0483(5) 1.3674(4) 0.0272(9) Uani 1 1 d .
O10 O 0.1505(6) 1.1967(5) 0.5676(5) 0.0719(13) Uani 1 1 d D
O11 O 1.0955(17) 1.6204(15) 1.6611(13) 0.039(3) Uani 0.30 1 d PU
O11' O 1.083(3) 1.562(2) 1.620(2) 0.045(5) Uani 0.20 1 d PU
H1A H 0.029(4) 1.200(4) 0.532(3) 0.080 Uiso 1 1 d D
H1B H 0.128(7) 1.109(2) 0.588(3) 0.080 Uiso 1 1 d D
H99 H 0.184(5) 0.978(5) 0.745(3) 0.035(13) Uiso 1 1 d D
H98 H 0.025(3) 0.919(4) 0.772(4) 0.032(13) Uiso 1 1 d D
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 '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
O7 La1 O3 90.38(11) . 2_677
O7 La1 O9 142.58(12) . .
O3 La1 O9 79.55(10) 2_677 .
O7 La1 O6 75.68(11) . .
O3 La1 O6 73.54(9) 2_677 .
O9 La1 O6 133.22(10) . .
O7 La1 O1 69.12(11) . 2_677
O3 La1 O1 69.31(9) 2_677 2_677
O9 La1 O1 73.62(11) . 2_677
O6 La1 O1 127.62(10) . 2_677
O7 La1 O2 109.88(11) . .
O3 La1 O2 156.87(10) 2_677 .
O9 La1 O2 77.55(10) . .
O6 La1 O2 121.25(9) . .
O1 La1 O2 106.79(9) 2_677 .
O7 La1 O5 71.15(11) . .
O3 La1 O5 123.33(9) 2_677 .
O9 La1 O5 143.32(11) . .
O6 La1 O5 50.30(9) . .
O1 La1 O5 138.30(11) 2_677 .
O2 La1 O5 75.43(9) . .
O7 La1 O4 140.08(11) . 1_455
O3 La1 O4 109.10(9) 2_677 1_455
O9 La1 O4 76.63(11) . 1_455
O6 La1 O4 77.06(10) . 1_455
O1 La1 O4 149.98(10) 2_677 1_455
O2 La1 O4 62.27(9) . 1_455
O5 La1 O4 69.02(10) . 1_455
O7 La1 O3 138.45(10) . 1_455
O3 La1 O3 62.31(10) 2_677 1_455
O9 La1 O3 66.58(10) . 1_455
O6 La1 O3 67.13(9) . 1_455
O1 La1 O3 121.07(9) 2_677 1_455
O2 La1 O3 104.95(8) . 1_455
O5 La1 O3 97.15(9) . 1_455
O4 La1 O3 46.87(8) 1_455 1_455
O7 La1 O1 78.78(10) . .
O3 La1 O1 132.50(9) 2_677 .
O9 La1 O1 81.90(10) . .
O6 La1 O1 143.49(10) . .
O1 La1 O1 63.58(10) 2_677 .
O2 La1 O1 46.56(8) . .
O5 La1 O1 96.77(9) . .
O4 La1 O1 108.44(8) 1_455 .
O3 La1 O1 142.77(8) 1_455 .
O7 La1 C6 71.04(12) . .
O3 La1 C6 98.43(11) 2_677 .
O9 La1 C6 145.79(11) . .
O6 La1 C6 25.21(10) . .
O1 La1 C6 138.00(10) 2_677 .
O2 La1 C6 98.67(11) . .
O5 La1 C6 25.10(10) . .
O4 La1 C6 71.82(10) 1_455 .
O3 La1 C6 82.11(10) 1_455 .
O1 La1 C6 120.34(11) . .
O7 La1 C3 96.78(11) . .
O3 La1 C3 148.09(10) 2_677 .
O9 La1 C3 75.93(10) . .
O6 La1 C3 138.36(10) . .
O1 La1 C3 84.28(10) 2_677 .
O2 La1 C3 23.25(9) . .
O5 La1 C3 88.27(10) . .
O4 La1 C3 84.79(9) 1_455 .
O3 La1 C3 123.23(9) 1_455 .
O1 La1 C3 23.64(9) . .
C6 La1 C3 113.33(11) . .
O10 K1 O5 93.88(13) . 2_687
O10 K1 O2 152.48(13) . 2_687
O5 K1 O2 70.94(9) 2_687 2_687
O10 K1 O2 103.87(13) . .
O5 K1 O2 133.95(10) 2_687 .
O2 K1 O2 103.09(8) 2_687 .
O10 K1 O4 107.23(13) . 1_455
O5 K1 O4 153.43(10) 2_687 1_455
O2 K1 O4 83.15(9) 2_687 1_455
O2 K1 O4 56.90(8) . 1_455
O10 K1 N2 85.17(14) . 1_455
O5 K1 N2 110.64(10) 2_687 1_455
O2 K1 N2 79.36(10) 2_687 1_455
O2 K1 N2 112.90(9) . 1_455
O4 K1 N2 57.00(9) 1_455 1_455
O10 K1 N1 82.19(13) . .
O5 K1 N1 86.25(10) 2_687 .
O2 K1 N1 118.23(10) 2_687 .
O2 K1 N1 55.51(9) . .
O4 K1 N1 111.99(9) 1_455 .
N2 K1 N1 159.57(11) 1_455 .
O10 K1 O4 138.39(13) . 2_787
O5 K1 O4 61.45(9) 2_687 2_787
O2 K1 O4 54.11(8) 2_687 2_787
O2 K1 O4 77.92(8) . 2_787
O4 K1 O4 107.91(7) 1_455 2_787
N2 K1 O4 133.29(10) 1_455 2_787
N1 K1 O4 64.42(9) . 2_787
O10 K1 K1 154.52(12) . 2_687
O5 K1 K1 107.47(8) 2_687 2_687
O2 K1 K1 51.96(7) 2_687 2_687
O2 K1 K1 51.13(7) . 2_687
O4 K1 K1 57.53(7) 1_455 2_687
N2 K1 K1 99.62(8) 1_455 2_687
N1 K1 K1 85.43(8) . 2_687
O4 K1 K1 50.37(6) 2_787 2_687
O10 K1 La1 130.24(11) . 2_687
O5 K1 La1 36.60(6) 2_687 2_687
O2 K1 La1 36.94(6) 2_687 2_687
O2 K1 La1 115.30(7) . 2_687
O4 K1 La1 119.31(7) 1_455 2_687
N2 K1 La1 105.16(8) 1_455 2_687
N1 K1 La1 95.25(7) . 2_687
O4 K1 La1 38.94(5) 2_787 2_687
K1 K1 La1 72.94(3) 2_687 2_687
O10 K1 H1A 18.4(5) . .
O5 K1 H1A 91.8(10) 2_687 .
O2 K1 H1A 135.6(5) 2_687 .
O2 K1 H1A 117.3(8) . .
O4 K1 H1A 103.1(11) 1_455 .
N2 K1 H1A 68.8(7) 1_455 .
N1 K1 H1A 100.3(6) . .
O4 K1 H1A 148.7(10) 2_787 .
K1 K1 H1A 160.3(11) 2_687 .
La1 K1 H1A 124.6(9) 2_687 .
O10 K1 H1B 18.0(5) . .
O5 K1 H1B 111.0(6) 2_687 .
O2 K1 H1B 163.0(10) 2_687 .
O2 K1 H1B 87.6(6) . .
O4 K1 H1B 92.0(8) 1_455 .
N2 K1 H1B 84.4(11) 1_455 .
N1 K1 H1B 78.7(10) . .
O4 K1 H1B 142.3(11) 2_787 .
K1 K1 H1B 137.0(5) 2_687 .
La1 K1 H1B 147.6(6) 2_687 .
H1A K1 H1B 30.2(4) . .
N1 S1 N2 98.48(18) . .
C3 O1 La1 141.5(3) . 2_677
C3 O1 La1 88.0(2) . .
La1 O1 La1 116.42(10) 2_677 .
C3 O2 La1 101.7(2) . .
C3 O2 K1 132.8(3) . 2_687
La1 O2 K1 102.37(10) . 2_687
C3 O2 K1 125.0(3) . .
La1 O2 K1 116.67(10) . .
K1 O2 K1 76.91(8) 2_687 .
C4 O3 La1 152.0(3) . 2_677
C4 O3 La1 90.3(2) . 1_655
La1 O3 La1 117.69(10) 2_677 1_655
C4 O4 La1 99.5(2) . 1_655
C4 O4 K1 117.0(2) . 1_655
La1 O4 K1 114.57(10) 1_655 1_655
C4 O4 K1 158.4(3) . 2_787
La1 O4 K1 93.40(8) 1_655 2_787
K1 O4 K1 72.09(7) 1_655 2_787
C6 O5 La1 92.9(2) . .
C6 O5 K1 134.9(3) . 2_687
La1 O5 K1 105.85(10) . 2_687
C6 O6 La1 95.5(2) . .
C8 O7 La1 163.5(3) . .
La1 O9 H99 128(3) . .
La1 O9 H98 116(3) . .
H99 O9 H98 110.2(18) . .
C1 N1 S1 108.3(3) . .
C1 N1 K1 120.4(3) . .
S1 N1 K1 130.22(17) . .
C2 N2 S1 107.4(3) . .
C2 N2 K1 117.5(3) . 1_655
S1 N2 K1 134.76(18) . 1_655
N1 C1 C2 112.2(3) . .
N1 C1 C3 117.0(3) . .
C2 C1 C3 130.7(3) . .
N2 C2 C1 113.5(3) . .
N2 C2 C4 116.4(3) . .
C1 C2 C4 130.1(3) . .
O1 C3 O2 122.0(4) . .
O1 C3 C1 121.5(3) . .
O2 C3 C1 116.5(3) . .
O1 C3 La1 68.4(2) . .
O2 C3 La1 55.01(19) . .
C1 C3 La1 164.2(3) . .
O4 C4 O3 123.1(4) . .
O4 C4 C2 117.7(3) . .
O3 C4 C2 119.1(4) . .
O4 C4 La1 57.3(2) . 1_655
O3 C4 La1 66.0(2) . 1_655
C2 C4 La1 170.1(3) . 1_655
C5 C5 C6 122.9(5) 2_688 .
C5 C5 H5 118.5 2_688 .
C6 C5 H5 118.5 . .
O5 C6 O6 121.2(4) . .
O5 C6 C5 120.9(4) . .
O6 C6 C5 117.9(4) . .
O5 C6 La1 62.0(2) . .
O6 C6 La1 59.3(2) . .
C5 C6 La1 175.9(3) . .
C7 C7 C8 123.8(5) 2_678 .
C7 C7 H7 118.1 2_678 .
C8 C7 H7 118.1 . .
O8 C8 O7 122.8(4) . .
O8 C8 C7 120.0(4) . .
O7 C8 C7 117.2(4) . .
K1 O10 H1A 102.8(15) . .
K1 O10 H1B 103.4(16) . .
H1A O10 H1B 109(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
La1 O7 2.411(3) .
La1 O3 2.475(3) 2_677
La1 O9 2.517(3) .
La1 O6 2.559(3) .
La1 O1 2.586(3) 2_677
La1 O2 2.600(3) .
La1 O5 2.620(3) .
La1 O4 2.661(3) 1_455
La1 O3 2.851(3) 1_455
La1 O1 2.890(3) .
La1 C6 2.963(4) .
La1 C3 3.107(4) .
K1 O10 2.627(5) .
K1 O5 2.677(3) 2_687
K1 O2 2.821(3) 2_687
K1 O2 2.854(3) .
K1 O4 2.857(3) 1_455
K1 N2 2.950(4) 1_455
K1 N1 2.955(4) .
K1 O4 3.129(3) 2_787
K1 K1 3.529(2) 2_687
K1 La1 4.2263(11) 2_687
K1 H1A 3.00(2) .
K1 H1B 2.99(2) .
S1 N1 1.620(4) .
S1 N2 1.627(4) .
O1 C3 1.247(5) .
O1 La1 2.586(3) 2_677
O2 C3 1.253(5) .
O2 K1 2.821(3) 2_687
O3 C4 1.253(5) .
O3 La1 2.475(3) 2_677
O3 La1 2.851(3) 1_655
O4 C4 1.248(5) .
O4 La1 2.661(3) 1_655
O4 K1 2.857(3) 1_655
O4 K1 3.129(3) 2_787
O5 C6 1.258(5) .
O5 K1 2.677(3) 2_687
O6 C6 1.268(5) .
O7 C8 1.256(5) .
O8 C8 1.244(5) .
O9 H99 0.852(10) .
O9 H98 0.842(10) .
N1 C1 1.329(5) .
N2 C2 1.327(5) .
N2 K1 2.950(4) 1_655
C1 C2 1.426(5) .
C1 C3 1.503(5) .
C2 C4 1.506(5) .
C4 La1 3.119(4) 1_655
C5 C5 1.309(9) 2_688
C5 C6 1.487(6) .
C5 H5 0.9300 .
C7 C7 1.303(9) 2_678
C7 C8 1.488(6) .
C7 H7 0.9300 .
O10 H1A 0.972(19) .
O10 H1B 0.950(19) .
O11 O11' 0.62(2) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O10 H1A O8 0.972(19) 2.12(3) 2.858(6) 132(3) 1_454
O10 H1B O8 0.950(19) 2.10(4) 2.851(6) 135(5) 2_677
