#------------------------------------------------------------------------------
#$Date: 2019-11-24 23:11:30 +0200 (Sun, 24 Nov 2019) $
#$Revision: 239698 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/70/4517019.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_4517019
loop_
_publ_author_name
'Senthilkumar, S.'
'Goswami, Ranadip'
'Obasi, Nnamdi Lawrence'
'Neogi, Subhadip'
_publ_section_title
;
 Construction of Pillar-Layer Metal--Organic Frameworks for CO2 Adsorption
 under Humid Climate: High Selectivity and Sensitive Detection of Picric
 Acid in Water
;
_journal_issue                   12
_journal_name_full               'ACS Sustainable Chemistry & Engineering'
_journal_page_first              11307
_journal_paper_doi               10.1021/acssuschemeng.7b02087
_journal_volume                  5
_journal_year                    2017
_chemical_formula_moiety         'C6 H2 N3 O7, 0.5(C10 H10 N4)'
_chemical_formula_sum            'C11 H7 N5 O7'
_chemical_formula_weight         321.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 97.599(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.535(2)
_cell_length_b                   19.583(9)
_cell_length_c                   11.673(5)
_cell_measurement_reflns_used    446
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.23
_cell_measurement_theta_min      2.73
_cell_volume                     1254.1(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_pressure         101.3
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0889
_diffrn_reflns_av_unetI/netI     0.1304
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5361
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.994
_diffrn_reflns_theta_min         2.044
_diffrn_source                   'X-ray tube'
_diffrn_source_type              'SMART Bruker'
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_description       needles
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.008(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2425
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0824P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1652
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1260
_reflns_number_total             2425
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            sc7b02087_si_002.cif
_cod_data_source_block           C:\CC1new\work\solve1_a
_cod_original_cell_volume        1254.2(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4517019
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.971
_shelx_estimated_absorpt_t_max   0.988
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1A O -0.3925(7) 0.6918(10) 0.4319(15) 0.033(2) Uani 0.76(5) 1 d D . P A 1
N1A N -0.1666(6) 0.69323(19) 0.4468(4) 0.0307(11) Uani 1 1 d D . . . .
C1A C 0.1844(8) 0.6751(2) 0.6013(4) 0.0204(11) Uani 1 1 d . . . . .
O2A O -0.043(3) 0.7301(10) 0.3910(12) 0.054(3) Uani 0.76(5) 1 d D U P A 1
N2A N 0.5384(6) 0.63645(15) 0.7447(3) 0.0247(10) Uani 1 1 d D . . . .
C2A C 0.3064(8) 0.6233(2) 0.6766(4) 0.0200(11) Uani 1 1 d . . . . .
O3A O 0.6564(5) 0.68774(14) 0.7244(3) 0.0265(8) Uani 1 1 d D . . . .
N3A N -0.1246(5) 0.47881(18) 0.6536(3) 0.0281(11) Uani 1 1 d D . . . .
C3A C 0.2069(8) 0.5598(2) 0.6914(4) 0.0222(11) Uani 1 1 d . . . . .
H3A H 0.291533 0.527811 0.743198 0.027 Uiso 1 1 calc R U . . .
O4A O 0.6199(6) 0.59471(17) 0.8194(3) 0.0381(10) Uani 1 1 d D . . . .
C4A C -0.0156(8) 0.5429(2) 0.6306(4) 0.0217(11) Uani 1 1 d . . . . .
O5A O -0.0077(6) 0.43742(16) 0.7196(3) 0.0395(10) Uani 1 1 d D . . . .
C5A C -0.1376(8) 0.5874(2) 0.5498(4) 0.0216(11) Uani 1 1 d . . . . .
H5A H -0.289095 0.574961 0.506946 0.026 Uiso 1 1 calc R U . . .
O6A O -0.3342(5) 0.46686(17) 0.6068(3) 0.0385(10) Uani 1 1 d D . . . .
C6A C -0.0350(8) 0.6491(2) 0.5336(4) 0.0206(11) Uani 1 1 d . . . . .
O7A O 0.2472(6) 0.73565(16) 0.5980(3) 0.0310(9) Uani 1 1 d . . . . .
O1B O -0.379(3) 0.675(2) 0.414(4) 0.033(2) Uani 0.24(5) 1 d D . P A 2
H1B H 0.522(7) 0.7840(18) 0.623(5) 0.05(2) Uiso 1 1 d D . . . .
N1B N 0.6224(8) 0.8157(2) 0.6095(4) 0.0251(10) Uani 1 1 d D . . . .
O2B O -0.084(8) 0.7465(16) 0.410(4) 0.054(3) Uani 0.24(5) 1 d D U P A 2
N2B N 1.0459(7) 0.98067(18) 0.5391(3) 0.0221(9) Uani 1 1 d . . . . .
C2B C 0.5373(9) 0.8546(2) 0.5175(4) 0.0240(11) Uani 1 1 d . . . . .
H2B H 0.388077 0.843400 0.471394 0.029 Uiso 1 1 calc R U . . .
C3B C 0.6688(8) 0.9105(2) 0.4914(4) 0.0258(12) Uani 1 1 d . . . . .
H3B H 0.609644 0.939440 0.428545 0.031 Uiso 1 1 calc R U . . .
C4B C 0.8890(8) 0.9241(2) 0.5583(4) 0.0196(11) Uani 1 1 d . . . . .
C5B C 0.9709(9) 0.8830(2) 0.6506(4) 0.0248(12) Uani 1 1 d . . . . .
H5B H 1.122836 0.892088 0.696092 0.030 Uiso 1 1 calc R U . . .
C6B C 0.8311(8) 0.8287(2) 0.6764(4) 0.0241(11) Uani 1 1 d . . . . .
H6B H 0.882840 0.800633 0.741468 0.029 Uiso 1 1 calc R U . . .
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
_geom_angle_site_symmetry_1
O2A N1A O1A 124.0(10) .
O2B N1A O1B 121(3) .
O2A N1A C6A 116.9(8) .
O2B N1A C6A 125(2) .
O1A N1A C6A 119.2(8) .
O1B N1A C6A 114(2) .
O7A C1A C2A 125.5(4) .
O7A C1A C6A 122.5(4) .
C2A C1A C6A 111.9(4) .
O4A N2A O3A 121.2(4) .
O4A N2A C2A 119.1(3) .
O3A N2A C2A 119.6(3) .
C3A C2A N2A 115.7(4) .
C3A C2A C1A 123.0(4) .
N2A C2A C1A 121.3(4) .
O6A N3A O5A 122.2(4) .
O6A N3A C4A 118.4(3) .
O5A N3A C4A 119.4(3) .
C4A C3A C2A 119.7(4) .
C4A C3A H3A 120.1 .
C2A C3A H3A 120.1 .
C3A C4A C5A 121.3(4) .
C3A C4A N3A 118.9(4) .
C5A C4A N3A 119.8(4) .
C6A C5A C4A 118.5(4) .
C6A C5A H5A 120.7 .
C4A C5A H5A 120.7 .
C5A C6A C1A 124.8(4) .
C5A C6A N1A 116.5(4) .
C1A C6A N1A 118.6(4) .
C6B N1B C2B 122.9(4) .
C6B N1B H1B 124(4) .
C2B N1B H1B 113(4) .
N2B N2B C4B 112.7(5) 3_776
N1B C2B C3B 119.2(5) .
N1B C2B H2B 120.4 .
C3B C2B H2B 120.4 .
C2B C3B C4B 118.8(4) .
C2B C3B H3B 120.6 .
C4B C3B H3B 120.6 .
C5B C4B C3B 120.3(4) .
C5B C4B N2B 115.4(4) .
C3B C4B N2B 124.3(4) .
C6B C5B C4B 119.3(4) .
C6B C5B H5B 120.3 .
C4B C5B H5B 120.3 .
N1B C6B C5B 119.4(5) .
N1B C6B H6B 120.3 .
C5B C6B H6B 120.3 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1A N1A 1.240(2) .
N1A O2A 1.239(2) .
N1A O2B 1.240(2) .
N1A O1B 1.240(2) .
N1A C6A 1.452(6) .
C1A O7A 1.237(5) .
C1A C2A 1.449(6) .
C1A C6A 1.451(6) .
N2A O4A 1.2366(19) .
N2A O3A 1.2378(19) .
N2A C2A 1.441(5) .
C2A C3A 1.381(6) .
N3A O6A 1.238(2) .
N3A O5A 1.2392(19) .
N3A C4A 1.434(6) .
C3A C4A 1.378(6) .
C3A H3A 0.9500 .
C4A C5A 1.391(6) .
C5A C6A 1.359(6) .
C5A H5A 0.9500 .
N1B C6B 1.331(6) .
N1B C2B 1.350(6) .
N1B H1B 0.860(2) .
N2B N2B 1.242(7) 3_776
N2B C4B 1.442(5) .
C2B C3B 1.371(6) .
C2B H2B 0.9500 .
C3B C4B 1.384(6) .
C3B H3B 0.9500 .
C4B C5B 1.373(6) .
C5B C6B 1.373(6) .
C5B H5B 0.9500 .
C6B H6B 0.9500 .
