#------------------------------------------------------------------------------
#$Date: 2017-06-22 03:33:54 +0300 (Thu, 22 Jun 2017) $
#$Revision: 198055 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/03/7120314.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_7120314
loop_
_publ_author_name
'McDonald, Kyle Andrew'
'Ko, Nakeun'
'Noh, Kyungkyou'
'Bennion, Jonathan C.'
'Kim, Jaheon'
'Matzger, Adam'
_publ_section_title
;
 Thermal Decomposition Pathways of Nitro-functionalized Metal-Organic
 Frameworks
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC03354K
_journal_year                    2017
_chemical_compound_source
'copper nitrate, tetranitrobiphenyl dicarboxylic acid'
_chemical_formula_moiety         'C14 H6 Cu N4 O13 [+ solvent]'
_chemical_formula_sum            'C14 H6 Cu N4 O13'
_chemical_formula_weight         501.77
_chemical_melting_point          ?
_chemical_name_common            CuNbO-1
_chemical_name_systematic        CuNbO-1
_chemical_properties_physical    ', Moisture-sensitive'
_space_group_crystal_system      cubic
_space_group_IT_number           229
_space_group_name_Hall           '-I 4 2 3'
_space_group_name_H-M_alt        'I m -3 m'
_symmetry_space_group_name_Hall  '-I 4 2 3'
_symmetry_space_group_name_H-M   'I m -3 m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-01 deposited with the CCDC.
2017-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   30.261(4)
_cell_length_b                   30.261(4)
_cell_length_c                   30.261(4)
_cell_measurement_reflns_used    20215
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      32.058
_cell_measurement_theta_min      2.087
_cell_volume                     27711(6)
_computing_cell_refinement
;
HKL3000SM (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
PAL BL2D-SMDC (Shin et al., 2016a)
;
_computing_data_reduction
;
HKL3000SM (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'ADSC Q210 CCD area-detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.900
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_unetI/netI     0.0098
_diffrn_reflns_Laue_measured_fraction_full 0.950
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            20215
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        32.058
_diffrn_reflns_theta_max         32.058
_diffrn_reflns_theta_min         2.087
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.472
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.361
_exptl_crystal_description       block
_exptl_crystal_F_000             3012
_exptl_crystal_recrystallization_method 'solvothermal reaction in DMA'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.028
_refine_ls_extinction_coef       0.0046(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014)'
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         2192
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0777
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2517
_refine_ls_wR_factor_ref         0.2620
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1666
_reflns_number_total             2192
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cc03354k3.cif
_cod_data_source_block           CuNbO-1_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'none' was changed to '?' - the value
is undefined or not given.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        27711(10)
_cod_database_code               7120314
_shelx_shelxl_version_number     2014/7
_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   0.871
_shelx_estimated_absorpt_t_max   0.911
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, z+1/2, -y+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'x+1/2, -z+1/2, y+1/2'
'z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z+1/2, x+1/2, y+1/2'
'z+1/2, x+1/2, -y+1/2'
'z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z+1/2, x+1/2'
'-y+1/2, z+1/2, x+1/2'
'y+1/2, z+1/2, -x+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'z+1/2, y+1/2, x+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
Cu1 Cu 0.5000 0.5000 0.04475(3) 0.1529(6) Uani 1 8 d DS T P
O1 O 0.5000 0.5000 0.1143(3) 0.227(2) Uani 1 8 d DS T P
H1 H 0.4816(6) 0.4816(6) 0.1254(8) 0.272 Uiso 0.5 2 d DS U P
O2 O 0.43548(8) 0.5000 0.03735(11) 0.1808(10) Uani 1 2 d S T P
C1 C 0.27538(15) 0.5000 0.0000 0.218(2) Uani 1 4 d S T P
C2 C 0.29972(15) 0.5000 0.03834(19) 0.2212(19) Uani 1 2 d S T P
C3 C 0.34449(16) 0.5000 0.03811(16) 0.2108(18) Uani 1 2 d S T P
H3 H 0.3596 0.5000 0.0652 0.253 Uiso 1 2 calc R U P
C4 C 0.36834(13) 0.5000 0.0000 0.1846(18) Uani 1 4 d S T P
C5 C 0.41755(13) 0.5000 0.0000 0.1735(17) Uani 1 4 d S T P
N1 N 0.27692(16) 0.5000 0.0808(3) 0.316(3) Uani 1 2 d S T P
O3 O 0.24156(16) 0.5000 0.0847(2) 0.525(5) Uani 1 2 d S T P
O4 O 0.29591(18) 0.5000 0.1114(2) 0.425(5) Uani 1 2 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0060 0.0030 '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 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0190 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.1510 1.9490 '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
O2 Cu1 O2 166.92(19) 62 61_665
O2 Cu1 O2 89.26(2) 62 2_665
O2 Cu1 O2 89.26(2) 61_665 2_665
O2 Cu1 O2 89.26(2) 62 .
O2 Cu1 O2 89.26(2) 61_665 .
O2 Cu1 O2 166.92(19) 2_665 .
O2 Cu1 O1 96.54(10) 62 .
O2 Cu1 O1 96.54(10) 61_665 .
O2 Cu1 O1 96.54(10) 2_665 .
O2 Cu1 O1 96.54(10) . .
O2 Cu1 Cu1 83.46(10) 62 49_665
O2 Cu1 Cu1 83.46(10) 61_665 49_665
O2 Cu1 Cu1 83.46(10) 2_665 49_665
O2 Cu1 Cu1 83.46(10) . 49_665
O1 Cu1 Cu1 180.0 . 49_665
C5 O2 Cu1 122.2(3) . .
C2 C1 C2 115.2(5) 50 .
C2 C1 C1 122.4(3) 50 89_554
C2 C1 C1 122.4(3) . 89_554
C3 C2 C1 122.1(5) . .
C3 C2 N1 118.5(5) . .
C1 C2 N1 119.4(5) . .
C2 C3 C4 122.3(5) . .
C3 C4 C3 115.9(5) 50 .
C3 C4 C5 122.0(2) 50 .
C3 C4 C5 122.0(2) . .
O2 C5 O2 128.7(4) . 50
O2 C5 C4 115.6(2) . .
O2 C5 C4 115.6(2) 50 .
O4 N1 O3 115.6(8) . .
O4 N1 C2 119.9(6) . .
O3 N1 C2 124.5(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O2 1.965(2) 62
Cu1 O2 1.965(2) 61_665
Cu1 O2 1.965(2) 2_665
Cu1 O2 1.965(2) .
Cu1 O1 2.104(8) .
Cu1 Cu1 2.7084(17) 49_665
O2 C5 1.254(3) .
C1 C2 1.374(6) 50
C1 C2 1.374(6) .
C1 C1 1.536(9) 89_554
C2 C3 1.355(7) .
C2 N1 1.459(7) .
C3 C4 1.361(5) .
C4 C3 1.361(5) 50
C4 C5 1.489(6) .
C5 O2 1.254(3) 50
N1 O4 1.089(7) .
N1 O3 1.076(6) .
