#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:47:14 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180518 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/87/7218730.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_7218730
loop_
_publ_author_name
'Chen, Wen-Bin'
'Li, Zhi-Xin'
'Ouyang, Zhi-Jian'
'Lin, Wen-Ning'
'Yang, Liu'
'Dong, Wen'
_publ_section_title
;
 Syntheses, Supramolecular Structures, Magnetic and Photochromic
 Properties of Six Lanthanide Complexes Based on 5-Azotetrazolyl Salicylic
 Acid Ligand
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA09951F
_journal_year                    2014
_chemical_formula_sum            'C16 H17 Gd N12 O10'
_chemical_formula_weight         694.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 105.473(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.3059(18)
_cell_length_b                   14.2088(16)
_cell_length_c                   10.0240(9)
_cell_measurement_reflns_used    5863
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.93
_cell_volume                     2238.3(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_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      296(2)
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8969
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    3.048
_exptl_absorpt_correction_T_max  0.633
_exptl_absorpt_correction_T_min  0.435
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.061
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1364.0
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.078
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.042(3)
_refine_ls_extinction_coef       0.00013(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         5107
_refine_ls_number_restraints     261
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0258P)²+9.1432P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0642
_reflns_number_gt                3852
_reflns_number_total             5107
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra09951f2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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      Cc
_cod_database_code               7218730
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'
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
Gd1 Gd 0.15328(13) 0.027608(13) 0.62151(17) 0.02669(8) Uani 1 1 d .
N10 N 0.4161(8) 0.3868(10) 1.7586(13) 0.049(2) Uani 1 1 d U
N11 N 0.3875(7) 0.3068(8) 1.7610(10) 0.0354(18) Uani 1 1 d U
H9 H 0.3918 0.2770 1.8372 0.043 Uiso 1 1 calc R
N5 N -0.0795(8) 0.3015(8) -0.5185(11) 0.038(2) Uani 1 1 d U
N12 N 0.3490(7) 0.2684(8) 1.6361(11) 0.0433(18) Uani 1 1 d U
N6 N -0.0412(7) 0.2826(8) -0.3862(11) 0.0437(19) Uani 1 1 d U
N3 N -0.0961(5) 0.4315(5) -0.4124(7) 0.0409(16) Uani 1 1 d U
N1 N 0.0015(8) 0.3052(8) -0.1179(11) 0.041(2) Uani 1 1 d U
N4 N -0.1113(8) 0.3916(9) -0.5270(13) 0.047(2) Uani 1 1 d U
N2 N -0.0284(7) 0.3773(8) -0.1766(12) 0.0448(18) Uani 1 1 d U
N9 N 0.3973(6) 0.4109(6) 1.6189(9) 0.0522(17) Uani 1 1 d U
N13 N 0.3146(7) 0.3627(8) 1.3237(9) 0.0298(17) Uani 0.50 1 d PU
N14 N 0.3006(13) 0.3087(14) 1.3469(18) 0.027(2) Uani 0.50 1 d PU
N7 N 0.3151(12) 0.2947(13) 1.3983(16) 0.036(2) Uani 0.50 1 d PU
N8 N 0.3277(13) 0.3811(16) 1.420(2) 0.033(2) Uani 0.50 1 d PU
C1 C 0.0818(7) 0.2485(8) 0.2623(11) 0.026(3) Uani 1 1 d .
C7 C 0.1068(7) 0.1538(9) 0.3296(11) 0.029(3) Uani 1 1 d .
C6 C 0.0539(9) 0.2470(10) 0.1172(14) 0.036(3) Uani 1 1 d U
H2 H 0.0525 0.1914 0.0677 0.043 Uiso 1 1 calc R
C5 C 0.0279(9) 0.3337(11) 0.0493(13) 0.049(3) Uani 1 1 d U
C2 C 0.0870(8) 0.3288(10) 0.3269(12) 0.041(3) Uani 1 1 d .
C4 C 0.0332(8) 0.4172(9) 0.1264(13) 0.062(3) Uani 1 1 d U
H3 H 0.0113 0.4729 0.0822 0.074 Uiso 1 1 calc R
C3 C 0.0668(13) 0.4171(10) 0.2522(17) 0.066(5) Uani 1 1 d .
H4 H 0.0792 0.4738 0.2996 0.079 Uiso 1 1 calc R
C8 C -0.0569(7) 0.3686(5) -0.3252(9) 0.033(2) Uani 1 1 d .
C9 C 0.2246(7) 0.2450(8) 0.9861(11) 0.024(3) Uani 1 1 d .
C14 C 0.2543(8) 0.2472(9) 1.1293(12) 0.028(3) Uani 1 1 d .
H8 H 0.2617 0.1897 1.1751 0.033 Uiso 1 1 calc R
C16 C 0.3559(6) 0.3345(9) 1.5528(9) 0.051(3) Uani 1 1 d U
C11 C 0.2387(11) 0.4145(10) 0.9890(19) 0.065(5) Uani 1 1 d U
H6 H 0.2384 0.4725 0.9458 0.078 Uiso 1 1 calc R
C13 C 0.2729(8) 0.3235(10) 1.2063(12) 0.036(2) Uani 1 1 d .
C10 C 0.2187(9) 0.3346(8) 0.9115(14) 0.036(3) Uani 1 1 d .
C12 C 0.2613(7) 0.4085(7) 1.1447(10) 0.041(2) Uani 1 1 d U
H7 H 0.2672 0.4631 1.1977 0.049 Uiso 1 1 calc R
C15 C 0.2006(7) 0.1576(8) 0.9106(12) 0.025(3) Uani 1 1 d .
O4 O 0.1928(7) 0.0837(6) 0.9838(11) 0.040(2) Uani 1 1 d .
O7 O 0.0173(9) -0.0265(6) 0.4500(13) 0.062(4) Uani 1 1 d .
O10 O 0.2788(7) -0.0293(5) 0.7943(11) 0.0324(19) Uani 1 1 d .
O5 O 0.1890(6) 0.1566(7) 0.7795(9) 0.039(2) Uani 1 1 d .
O2 O 0.1185(7) 0.1521(6) 0.4605(9) 0.037(2) Uani 1 1 d .
O9 O 0.2867(7) 0.0854(6) 0.5713(11) 0.045(3) Uani 1 1 d .
H9A H 0.2874 0.0782 0.4771 0.067 Uiso 1 1 d R
H9B H 0.2971 0.1506 0.5902 0.067 Uiso 1 1 d R
O8 O 0.0218(6) 0.0889(7) 0.6713(11) 0.045(3) Uani 1 1 d .
H8A H -0.0178 0.0439 0.6637 0.067 Uiso 1 1 d R
H8B H 0.0327 0.1118 0.7576 0.067 Uiso 1 1 d R
O3 O 0.1157(8) 0.3381(8) 0.4715(10) 0.056(3) Uani 1 1 d .
H1 H 0.1108 0.2875 0.5080 0.083 Uiso 1 1 calc R
O6 O 0.1949(8) 0.3395(8) 0.7796(11) 0.058(3) Uani 1 1 d .
H5 H 0.1769 0.2880 0.7477 0.088 Uiso 1 1 calc R
O1 O 0.1163(7) 0.0859(6) 0.2653(10) 0.039(2) Uani 1 1 d .
H7A H -0.0291 -0.0228 0.4746 0.058 Uiso 1 1 d R
H7B H 0.0118 0.0133 0.3850 0.058 Uiso 1 1 d R
H10A H 0.3127 0.0172 0.8198 0.058 Uiso 1 1 d R
H10B H 0.3140 -0.0734 0.7730 0.058 Uiso 1 1 d 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'
Gd Gd -0.1653 3.9035 '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
O4 Gd1 O1 93.18(12) 2_554 2
O4 Gd1 O2 99.2(3) 2_554 .
O1 Gd1 O2 151.8(4) 2 .
O4 Gd1 O5 150.1(4) 2_554 .
O1 Gd1 O5 100.2(3) 2 .
O2 Gd1 O5 81.37(12) . .
O4 Gd1 O10 83.2(4) 2_554 .
O1 Gd1 O10 68.9(4) 2 .
O2 Gd1 O10 137.5(3) . .
O5 Gd1 O10 76.9(3) . .
O4 Gd1 O8 139.1(4) 2_554 .
O1 Gd1 O8 74.9(3) 2 .
O2 Gd1 O8 79.2(3) . .
O5 Gd1 O8 70.7(4) . .
O10 Gd1 O8 125.4(4) . .
O4 Gd1 O9 73.0(3) 2_554 .
O1 Gd1 O9 136.9(4) 2 .
O2 Gd1 O9 71.3(4) . .
O5 Gd1 O9 79.0(3) . .
O10 Gd1 O9 69.0(4) . .
O8 Gd1 O9 140.30(12) . .
O4 Gd1 O7 73.7(4) 2_554 .
O1 Gd1 O7 83.5(4) 2 .
O2 Gd1 O7 75.9(3) . .
O5 Gd1 O7 134.1(4) . .
O10 Gd1 O7 142.84(14) . .
O8 Gd1 O7 66.2(4) . .
O9 Gd1 O7 127.9(4) . .
N11 N10 N9 105.3(11) . .
N10 N11 N12 116.0(11) . .
N10 N11 H9 122.0 . .
N12 N11 H9 122.0 . .
N6 N5 N4 108.5(11) . .
C16 N12 N11 101.9(11) . .
N5 N6 C8 99.4(9) . .
N4 N3 C8 104.5(9) . .
N2 N1 C5 104.2(11) . .
N3 N4 N5 112.8(11) . .
N1 N2 C8 113.9(11) . .
C16 N9 N10 104.0(9) . .
N14 N13 N8 88.6(19) . .
N14 N13 N7 22.6(15) . .
N8 N13 N7 68.9(16) . .
N14 N13 C13 75.6(16) . .
N8 N13 C13 158.7(16) . .
N7 N13 C13 97.5(13) . .
N14 N13 C12 118.8(16) . .
N8 N13 C12 141.1(16) . .
N7 N13 C12 141.4(12) . .
C13 N13 C12 45.5(7) . .
N7 N14 N13 121(4) . .
N7 N14 N8 76(3) . .
N13 N14 N8 49.4(15) . .
N7 N14 C13 165(4) . .
N13 N14 C13 67.7(13) . .
N8 N14 C13 115.7(17) . .
N14 N7 N13 37(3) . .
N14 N7 N8 79(3) . .
N13 N7 N8 45.9(11) . .
N14 N7 C16 138(4) . .
N13 N7 C16 104.1(13) . .
N8 N7 C16 59.0(12) . .
N14 N7 C13 11(3) . .
N13 N7 C13 43.1(8) . .
N8 N7 C13 87.8(13) . .
C16 N7 C13 146.8(13) . .
N13 N8 N7 65.2(17) . .
N13 N8 N14 41.9(13) . .
N7 N8 N14 24.9(10) . .
N13 N8 C16 136(2) . .
N7 N8 C16 73.0(13) . .
N14 N8 C16 97.8(16) . .
C2 C1 C6 119.2(10) . .
C2 C1 C7 125.7(10) . .
C6 C1 C7 115.0(11) . .
O1 C7 O2 122.4(11) . .
O1 C7 C1 122.5(11) . .
O2 C7 C1 115.1(10) . .
C1 C6 C5 117.2(13) . .
C1 C6 H2 121.4 . .
C5 C6 H2 121.4 . .
C4 C5 C6 120.3(12) . .
C4 C5 N1 136.0(10) . .
C6 C5 N1 103.7(12) . .
C1 C2 O3 123.6(11) . .
C1 C2 C3 121.6(11) . .
O3 C2 C3 114.7(12) . .
C3 C4 C5 120.3(12) . .
C3 C4 H3 119.8 . .
C5 C4 H3 119.8 . .
C4 C3 C2 120.4(14) . .
C4 C3 H4 119.8 . .
C2 C3 H4 119.8 . .
N3 C8 N6 114.7(9) . .
N3 C8 N2 127.2(9) . .
N6 C8 N2 118.2(9) . .
C14 C9 C15 122.0(10) . .
C14 C9 C10 117.7(11) . .
C15 C9 C10 120.3(10) . .
C13 C14 C9 125.9(12) . .
C13 C14 H8 117.0 . .
C9 C14 H8 117.0 . .
N12 C16 N9 112.8(9) . .
N12 C16 N8 150.9(14) . .
N9 C16 N8 94.4(12) . .
N12 C16 N7 106.4(11) . .
N9 C16 N7 140.6(11) . .
N8 C16 N7 48.0(12) . .
C10 C11 C12 119.8(12) . .
C10 C11 H6 120.1 . .
C12 C11 H6 120.1 . .
N13 C13 C14 148.7(14) . .
N13 C13 C12 90.4(11) . .
C14 C13 C12 119.1(11) . .
N13 C13 N14 36.7(10) . .
C14 C13 N14 115.8(14) . .
C12 C13 N14 125.1(13) . .
N13 C13 N7 39.4(8) . .
C14 C13 N7 112.2(12) . .
C12 C13 N7 128.7(11) . .
N14 C13 N7 4.2(11) . .
O6 C10 C11 120.3(11) . .
O6 C10 C9 122.4(11) . .
C11 C10 C9 117.3(12) . .
C13 C12 C11 119.5(10) . .
C13 C12 N13 44.1(7) . .
C11 C12 N13 157.9(10) . .
C13 C12 H7 120.3 . .
C11 C12 H7 120.3 . .
N13 C12 H7 78.1 . .
O5 C15 O4 124.0(11) . .
O5 C15 C9 119.4(10) . .
O4 C15 C9 116.6(10) . .
C15 O4 Gd1 166.9(9) . 2
Gd1 O7 H7A 117.7 . .
Gd1 O7 H7B 102.2 . .
H7A O7 H7B 104.9 . .
Gd1 O10 H10A 108.0 . .
Gd1 O10 H10B 121.5 . .
H10A O10 H10B 101.7 . .
C15 O5 Gd1 129.3(8) . .
C7 O2 Gd1 131.3(8) . .
Gd1 O9 H9A 113.9 . .
Gd1 O9 H9B 113.5 . .
H9A O9 H9B 104.6 . .
Gd1 O8 H8A 111.9 . .
Gd1 O8 H8B 111.1 . .
H8A O8 H8B 107.2 . .
C2 O3 H1 109.5 . .
C10 O6 H5 109.5 . .
C7 O1 Gd1 168.3(9) . 2_554
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Gd1 O4 2.301(9) 2_554
Gd1 O1 2.347(9) 2
Gd1 O2 2.360(9) .
Gd1 O5 2.391(9) .
Gd1 O10 2.439(10) .
Gd1 O8 2.485(10) .
Gd1 O9 2.499(11) .
Gd1 O7 2.536(13) .
N10 N11 1.231(18) .
N10 N9 1.394(14) .
N11 N12 1.356(16) .
N11 H9 0.8600 .
N5 N6 1.334(15) .
N5 N4 1.376(18) .
N12 C16 1.281(15) .
N6 C8 1.421(14) .
N3 N4 1.245(14) .
N3 C8 1.294(11) .
N1 N2 1.217(16) .
N1 C5 1.665(17) .
N2 C8 1.442(14) .
N9 C16 1.354(14) .
N13 N14 0.85(2) .
N13 N8 0.97(2) .
N13 N7 1.221(19) .
N13 C13 1.315(15) .
N13 C12 1.889(14) .
N14 N7 0.544(18) .
N14 N8 1.27(3) .
N14 C13 1.38(2) .
N7 N8 1.25(3) .
N7 C16 1.616(18) .
N7 C13 1.908(19) .
N8 C16 1.45(2) .
C1 C2 1.304(18) .
C1 C6 1.403(17) .
C1 C7 1.512(16) .
C7 O1 1.192(15) .
C7 O2 1.274(14) .
C6 C5 1.42(2) .
C6 H2 0.9300 .
C5 C4 1.41(2) .
C2 O3 1.405(15) .
C2 C3 1.453(18) .
C4 C3 1.23(2) .
C4 H3 0.9300 .
C3 H4 0.9300 .
C9 C14 1.388(15) .
C9 C15 1.452(17) .
C9 C10 1.467(15) .
C14 C13 1.319(19) .
C14 H8 0.9300 .
C11 C10 1.37(2) .
C11 C12 1.51(2) .
C11 H6 0.9300 .
C13 C12 1.347(18) .
C10 O6 1.276(17) .
C12 H7 0.9300 .
C15 O5 1.277(15) .
C15 O4 1.307(15) .
O4 Gd1 2.301(9) 2
O7 H7A 0.8572 .
O7 H7B 0.8499 .
O10 H10A 0.8566 .
O10 H10B 0.9141 .
O9 H9A 0.9537 .
O9 H9B 0.9514 .
O8 H8A 0.8969 .
O8 H8B 0.8963 .
O3 H1 0.8200 .
O6 H5 0.8200 .
O1 Gd1 2.347(9) 2_554
