#------------------------------------------------------------------------------
#$Date: 2016-03-25 22:31:57 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180014 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/08/7030852.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_7030852
loop_
_publ_author_name
'Chen, Wen-Bin'
'Li, Zhi-Xin'
'Yu, Xin-Wei'
'Yang, Meng'
'Qiu, Yan-Xuan'
'Dong, Wen'
'Sun, Ya-Qiu'
_publ_section_title
;
 Syntheses, structures and properties of 5-azotetrazolyl salicylic acid
 and its dilanthanide complexes.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9090
_journal_page_last               9097
_journal_paper_doi               10.1039/c4dt00278d
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C8 H14 N6 O7'
_chemical_formula_weight         306.25
_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                 101.58(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.104(10)
_cell_length_b                   3.8044(13)
_cell_length_c                   27.047(9)
_cell_measurement_reflns_used    1610
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.77
_cell_measurement_theta_min      2.38
_cell_volume                     2732.2(17)
_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 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.0454
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            10622
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.961
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1280.0
_exptl_crystal_size_max          0.346
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0057(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         30135
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1192
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1324P)²+1.0209P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2087
_refine_ls_wR_factor_ref         0.2402
_reflns_number_gt                1730
_reflns_number_total             3135
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00278d2.cif
_cod_data_source_block           1
_cod_depositor_comments
;Adding full bibliography for 7030851--7030857.cif.

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      C2/c
_cod_database_code               7030852
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
N1 N 0.20667(9) 1.0190(8) 0.13317(9) 0.0341(7) Uani 1 1 d .
N2 N 0.25264(9) 1.0562(8) 0.15298(10) 0.0359(7) Uani 1 1 d .
N3 N 0.26639(10) 1.2868(8) 0.07240(10) 0.0377(7) Uani 1 1 d .
H1 H 0.2362 1.3480 0.0586 0.045 Uiso 1 1 calc R
N6 N 0.33120(9) 1.0813(8) 0.12684(10) 0.0376(7) Uani 1 1 d .
N4 N 0.30810(11) 1.3212(8) 0.05371(10) 0.0406(7) Uani 1 1 d .
N5 N 0.34690(10) 1.1960(8) 0.08588(10) 0.0401(7) Uani 1 1 d .
C6 C 0.12721(11) 0.8231(9) 0.14635(12) 0.0349(8) Uani 1 1 d .
H6 H 0.1185 0.7951 0.1115 0.042 Uiso 1 1 calc R
C5 C 0.17457(12) 0.9490(9) 0.16762(11) 0.0313(7) Uani 1 1 d .
C3 C 0.15391(12) 0.9204(10) 0.24906(12) 0.0392(8) Uani 1 1 d .
H3 H 0.1626 0.9556 0.2837 0.047 Uiso 1 1 calc R
C2 C 0.10611(12) 0.7865(9) 0.22777(12) 0.0343(8) Uani 1 1 d .
C1 C 0.09240(11) 0.7376(9) 0.17547(11) 0.0322(7) Uani 1 1 d .
C4 C 0.18791(11) 1.0000(9) 0.21968(12) 0.0350(8) Uani 1 1 d .
H4 H 0.2196 1.0870 0.2342 0.042 Uiso 1 1 calc R
C8 C 0.28204(11) 1.1357(9) 0.11749(11) 0.0327(8) Uani 1 1 d .
C7 C 0.04178(12) 0.5932(10) 0.15185(14) 0.0419(9) Uani 1 1 d D
O3 O 0.07396(9) 0.7099(8) 0.25817(9) 0.0506(8) Uani 1 1 d .
H5 H 0.0471 0.6424 0.2411 0.076 Uiso 1 1 calc R
O2 O 0.01100(9) 0.5524(8) 0.18091(10) 0.0545(8) Uani 1 1 d D
O1 O 0.03233(9) 0.5278(8) 0.10585(10) 0.0556(8) Uani 1 1 d D
O4 O 0.92443(11) 0.1539(9) 0.15283(12) 0.0626(9) Uani 1 1 d D
O5 O 0.09217(11) 0.2955(10) 0.03291(12) 0.0677(9) Uani 1 1 d D
O6 O 0.17809(11) 0.7208(9) 0.02910(11) 0.0604(8) Uani 1 1 d D
O7 O 0.03886(16) 0.9958(11) 0.94337(16) 0.0899(12) Uani 1 1 d D
H7 H 0.925(2) 0.015(15) 0.176(2) 0.135 Uiso 1 1 d D
H9 H 0.075(2) 0.331(19) 0.0538(17) 0.135 Uiso 1 1 d D
H10 H 0.077(2) 0.22(2) 0.0073(14) 0.135 Uiso 1 1 d D
H12 H 0.180(2) 0.860(15) 0.0533(19) 0.135 Uiso 1 1 d D
H11 H 0.1496(14) 0.621(16) 0.025(2) 0.135 Uiso 1 1 d D
H13 H 0.049(2) 0.798(9) 0.940(3) 0.135 Uiso 1 1 d D
H14 H 0.0102(13) 0.980(18) 0.949(3) 0.135 Uiso 1 1 d D
H2 H -0.0147(15) 0.417(15) 0.1687(12) 0.135 Uiso 1 1 d D
H8 H 0.8971(11) 0.263(11) 0.1481(17) 0.071(15) 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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N2 N1 C5 115.1(2)
N1 N2 C8 112.5(2)
N4 N3 C8 104.5(3)
N4 N3 H1 127.8
C8 N3 H1 127.8
C8 N6 N5 105.5(3)
N5 N4 N3 109.9(3)
N4 N5 N6 108.8(3)
C5 C6 C1 121.8(3)
C5 C6 H6 119.1
C1 C6 H6 119.1
C6 C5 C4 119.9(3)
C6 C5 N1 115.5(3)
C4 C5 N1 124.5(3)
C4 C3 C2 121.1(3)
C4 C3 H3 119.4
C2 C3 H3 119.4
O3 C2 C1 121.1(3)
O3 C2 C3 119.1(3)
C1 C2 C3 119.9(3)
C6 C1 C2 118.1(3)
C6 C1 C7 121.0(3)
C2 C1 C7 120.9(3)
C3 C4 C5 119.2(3)
C3 C4 H4 120.4
C5 C4 H4 120.4
N6 C8 N3 111.4(3)
N6 C8 N2 121.8(3)
N3 C8 N2 126.8(3)
O1 C7 O2 124.6(3)
O1 C7 C1 119.2(3)
O2 C7 C1 116.2(3)
C2 O3 H5 109.5
C7 O2 H2 114.3(15)
H7 O4 H8 109(3)
H9 O5 H10 113(4)
H12 O6 H11 106(3)
H13 O7 H14 108(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
N1 N2 1.261(4)
N1 C5 1.422(4)
N2 C8 1.398(4)
N3 N4 1.334(4)
N3 C8 1.338(4)
N3 H1 0.8600
N6 C8 1.322(4)
N6 N5 1.337(4)
N4 N5 1.312(4)
C6 C5 1.383(4)
C6 C1 1.384(4)
C6 H6 0.9300
C5 C4 1.395(4)
C3 C4 1.366(4)
C3 C2 1.404(5)
C3 H3 0.9300
C2 O3 1.344(4)
C2 C1 1.401(4)
C1 C7 1.497(4)
C4 H4 0.9300
C7 O1 1.244(4)
C7 O2 1.265(4)
O3 H5 0.8200
O2 H2 0.877(18)
O4 H7 0.82(2)
O4 H8 0.838(19)
O5 H9 0.808(19)
O5 H10 0.788(19)
O6 H12 0.84(2)
O6 H11 0.85(2)
O7 H13 0.81(2)
O7 H14 0.82(2)
