#------------------------------------------------------------------------------
#$Date: 2016-03-22 14:03:27 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178984 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/07/4120782.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_4120782
loop_
_publ_author_name
'Natalia B. Shustova'
'Anthony F. Cozzolino'
'Sebastian Reineke'
'Marc Baldo'
'Mircea Dincă'
_publ_section_title
;
 Selective Turn-On Ammonia Sensing Enabled by High-Temperature
 Fluorescence in Metal-Organic Frameworks with Open Metal Sites
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13326
_journal_page_last               13329
_journal_paper_doi               10.1021/ja407778a
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C8 H5 O6 N H4, H2O'
_chemical_formula_sum            'C8 H11 N O7'
_chemical_formula_weight         233.18
_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                101.161(2)
_cell_angle_beta                 110.6220(10)
_cell_angle_gamma                111.735(2)
_cell_formula_units_Z            2
_cell_length_a                   6.7456(5)
_cell_length_b                   9.0252(7)
_cell_length_c                   9.4246(7)
_cell_measurement_reflns_used    4696
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.53
_cell_measurement_theta_min      2.49
_cell_volume                     462.90(6)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2010)'
_computing_data_collection       'APEX2 v2010.7.0 (Bruker-AXS, 2010)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2010)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean '\f and \w scans'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       'φ and ω 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  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0191
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7965
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    0.149
_exptl_absorpt_correction_T_max  0.9926
_exptl_absorpt_correction_T_min  0.9852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            plate
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_description       colorless
_exptl_crystal_F_000             244
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         1868
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0360
_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)+(0.0524P)²+0.1986P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1075
_reflns_number_gt                1587
_reflns_number_total             1868
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja407778a_si_002.cif
_cod_data_source_block           c_a
_cod_database_code               4120782
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
C1 C 0.1729(3) 0.38281(19) 0.43486(18) 0.0121(3) Uani 1 1 d U
C2 C 0.1860(3) 0.52539(19) 0.39548(18) 0.0125(3) Uani 1 1 d U
H2 H 0.1090 0.5113 0.2841 0.015 Uiso 1 1 calc R
C3 C 0.3100(3) 0.68862(19) 0.51636(19) 0.0126(3) Uani 1 1 d U
C4 C 0.4275(3) 0.70930(18) 0.68076(18) 0.0114(3) Uani 1 1 d U
C5 C 0.4130(3) 0.56594(19) 0.71977(18) 0.0127(3) Uani 1 1 d U
H5 H 0.4896 0.5797 0.8310 0.015 Uiso 1 1 calc R
C6 C 0.2889(3) 0.40368(19) 0.59933(19) 0.0123(3) Uani 1 1 d U
C7 C 0.0361(3) 0.20709(19) 0.30524(18) 0.0130(3) Uani 1 1 d U
C8 C 0.5686(3) 0.88419(19) 0.81249(18) 0.0126(3) Uani 1 1 d U
H1 H -0.181(5) 0.065(4) 0.074(4) 0.079(10) Uiso 1 1 d .
H3 H 0.407(4) 0.922(3) 0.574(2) 0.053(7) Uiso 1 1 d D
H4 H 0.187(4) 0.167(3) 0.542(2) 0.058(8) Uiso 1 1 d D
H6 H 0.571(3) 0.324(3) 0.850(2) 0.045(7) Uiso 1 1 d D
H7 H 0.699(5) 0.295(3) 0.989(3) 0.067(9) Uiso 1 1 d D
H8 H 0.880(4) 0.625(2) 0.074(2) 0.037(6) Uiso 1 1 d D
H9 H 0.922(4) 0.760(3) 0.227(2) 0.049(7) Uiso 1 1 d D
H10 H 1.111(3) 0.808(3) 0.165(3) 0.048(7) Uiso 1 1 d D
H11 H 0.856(4) 0.789(3) 0.062(2) 0.034(6) Uiso 1 1 d D
N1 N 0.9436(2) 0.74597(17) 0.13193(16) 0.0152(3) Uani 1 1 d D
O1 O 0.0387(2) 0.08234(14) 0.33923(13) 0.0177(3) Uani 1 1 d U
O2 O -0.0837(2) 0.19649(14) 0.15776(13) 0.0165(3) Uani 1 1 d U
O3 O 0.3118(2) 0.82232(14) 0.46989(13) 0.0178(3) Uani 1 1 d DU
O4 O 0.2810(2) 0.26768(13) 0.64645(14) 0.0161(3) Uani 1 1 d DU
O5 O 0.6874(2) 0.89635(14) 0.95822(13) 0.0173(3) Uani 1 1 d U
O6 O 0.56865(19) 1.01012(13) 0.77615(13) 0.0154(3) Uani 1 1 d U
O7 O 0.7022(2) 0.38080(15) 0.95145(15) 0.0219(3) Uani 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
C2 C1 C6 119.55(14)
C2 C1 C7 121.07(14)
C6 C1 C7 119.38(14)
C1 C2 C3 121.07(14)
C1 C2 H2 119.5
C3 C2 H2 119.5
O3 C3 C2 118.15(14)
O3 C3 C4 122.61(13)
C2 C3 C4 119.24(14)
C5 C4 C3 119.49(13)
C5 C4 C8 120.25(14)
C3 C4 C8 120.26(13)
C6 C5 C4 121.13(14)
C6 C5 H5 119.4
C4 C5 H5 119.4
O4 C6 C5 118.09(14)
O4 C6 C1 122.40(13)
C5 C6 C1 119.50(14)
O1 C7 O2 123.47(13)
O1 C7 C1 120.95(14)
O2 C7 C1 115.58(13)
O6 C8 O5 123.40(13)
O6 C8 C4 119.33(13)
O5 C8 C4 117.26(13)
H8 N1 H9 108.5(19)
H8 N1 H10 111.4(19)
H9 N1 H10 108(2)
H8 N1 H11 108.7(18)
H9 N1 H11 109.5(19)
H10 N1 H11 110.6(19)
C7 O2 H1 110.2(15)
C3 O3 H3 103.7(15)
C6 O4 H4 104.1(15)
H6 O7 H7 103(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 C2 1.388(2)
C1 C6 1.405(2)
C1 C7 1.494(2)
C2 C3 1.391(2)
C2 H2 0.9500
C3 O3 1.3583(18)
C3 C4 1.406(2)
C4 C5 1.391(2)
C4 C8 1.495(2)
C5 C6 1.383(2)
C5 H5 0.9500
C6 O4 1.3732(18)
C7 O1 1.2332(19)
C7 O2 1.3016(19)
C8 O6 1.2488(18)
C8 O5 1.2812(18)
N1 H8 0.967(16)
N1 H9 0.949(16)
N1 H10 0.948(16)
N1 H11 0.963(16)
O2 H1 1.08(3)
O3 H3 0.989(17)
O4 H4 0.994(17)
O7 H6 0.917(17)
O7 H7 0.911(17)
