#------------------------------------------------------------------------------
#$Date: 2018-12-13 01:46:31 +0200 (Thu, 13 Dec 2018) $
#$Revision: 212561 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/19/7231985.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_7231985
loop_
_publ_author_name
'Lu, Jack'
'Zhang, Sheng'
'Wu, Shuo'
'Zhang, Wendou'
'Yang, Qi'
'Wei, Qing'
'Xie, Gang'
'Chen, Sanping'
'Gao, Sheng-li'
_publ_section_title
;
 A 3D solvent-free energetic metal-organic framework (EMOF) achieved by
 removing inclusion molecules from a new coordination polymer
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C8CE01803K
_journal_year                    2018
_chemical_formula_moiety         'C8 H4 Cu3 N16 Na O4'
_chemical_formula_sum            'C8 H4 Cu3 N16 Na O4'
_chemical_formula_weight         601.88
_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_Hall           '-I 4bd 2'
_space_group_name_H-M_alt        'I 41/a m d'
_symmetry_space_group_name_Hall  '-I 4bd 2'
_symmetry_space_group_name_H-M   'I 41/a m d :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-05-25
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-11-05 deposited with the CCDC.
2018-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.638(3)
_cell_length_b                   13.638(3)
_cell_length_c                   11.428(3)
_cell_measurement_reflns_used    586
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      22.36
_cell_measurement_theta_min      2.99
_cell_volume                     2125.6(9)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5475
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.244
_diffrn_reflns_theta_min         2.325
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.048
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6255
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0966 before and 0.0497 after correction.
The Ratio of minimum to maximum transmission is 0.8391.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     51
_refine_ls_number_reflns         585
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.250
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0827P)²+19.7884P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1657
_refine_ls_wR_factor_ref         0.1803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                429
_reflns_number_total             585
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce01803k2.cif
_cod_data_source_block           xb9535_sq
_cod_original_cell_volume        2125.6(11)
_cod_database_code               7231985
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.009 and
sigma for terminal atoms of 0.009
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/4, x+3/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+1/4, -x+1/4, z+3/4'
'x, -y, -z'
'y+1/4, x+3/4, -z+1/4'
'-x+1/2, y, -z+1/2'
'-y+1/4, -x+1/4, -z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+3/4, -x+3/4, z+5/4'
'x+1/2, -y+1/2, -z+1/2'
'y+3/4, x+5/4, -z+3/4'
'-x+1, y+1/2, -z+1'
'-y+3/4, -x+3/4, -z+5/4'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-1/4, x-1/4, -z-3/4'
'-x, y, z'
'-y-1/4, -x-3/4, z-1/4'
'x-1/2, -y, z-1/2'
'y-1/4, x-1/4, z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z+1/4'
'x, y+1/2, -z'
'-y+1/4, x+1/4, -z-1/4'
'-x+1/2, y+1/2, z+1/2'
'-y+1/4, -x-1/4, z+1/4'
'x, -y+1/2, z'
'y+1/4, x+1/4, z-1/4'
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 0.7500 0.3750 0.0349(7) Uani 1 8 d S T P
Cu2 Cu 0.5000 0.5000 0.5000 0.0413(6) Uani 1 4 d S T P
Na1 Na 0.5000 0.2500 0.1250 0.0383(18) Uani 1 8 d S T P
O1 O 0.5000 0.3717(6) 0.2599(6) 0.054(2) Uani 1 2 d S T P
N1 N 0.5000 0.5139(6) 0.1477(6) 0.0357(19) Uani 1 2 d S T P
N4 N 0.5000 0.4698(6) 0.0407(7) 0.043(2) Uani 1 2 d S T P
N2 N 0.5000 0.6230(6) 0.2878(7) 0.045(2) Uani 1 2 d S T P
N3 N 0.5000 0.5264(6) 0.3391(6) 0.038(2) Uani 1 2 d S T P
C1 C 0.5000 0.4599(8) 0.2527(8) 0.038(2) Uani 1 2 d S T P
C2 C 0.5000 0.6124(9) 0.1763(9) 0.050(3) Uani 1 2 d S T P
H2 H 0.5000 0.6636 0.1225 0.060 Uiso 1 2 calc RS 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 0.0033 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'
Cu Cu 0.3201 1.2651 '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'
Na Na 0.0362 0.0249 '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
_geom_angle_site_symmetry_3
N2 Cu1 N2 104.4(2) . 28_656
N2 Cu1 N2 120.2(5) 28_656 18_576
N2 Cu1 N2 104.4(2) . 18_576
N2 Cu1 N2 104.4(2) 28_656 11_564
N2 Cu1 N2 104.4(2) 18_576 11_564
N2 Cu1 N2 120.2(5) . 11_564
N3 Cu2 N3 180.0 17_666 .
O1 Na1 O1 117.58(19) 20_656 11_554
O1 Na1 O1 117.58(19) . 20_656
O1 Na1 O1 94.2(3) 20_656 26_565
O1 Na1 O1 94.2(3) . 11_554
O1 Na1 O1 117.58(19) . 26_565
O1 Na1 O1 117.58(19) 26_565 11_554
C1 O1 Na1 133.2(6) . .
N4 N1 C1 122.3(8) . .
N4 N1 C2 129.9(8) . .
C2 N1 C1 107.8(8) . .
N4 N4 N1 112.3(11) 17_665 .
N3 N2 Cu1 126.1(6) . .
C2 N2 Cu1 126.4(8) . .
C2 N2 N3 107.5(9) . .
N2 N3 Cu2 125.1(6) . .
C1 N3 Cu2 126.3(7) . .
C1 N3 N2 108.6(8) . .
O1 C1 N1 125.4(8) . .
O1 C1 N3 128.7(9) . .
N3 C1 N1 105.9(9) . .
N1 C2 H2 124.9 . .
N2 C2 N1 110.1(10) . .
N2 C2 H2 124.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N2 1.998(9) .
Cu1 N2 1.998(9) 18_576
Cu1 N2 1.998(9) 11_564
Cu1 N2 1.998(9) 28_656
Cu2 N3 1.874(7) 17_666
Cu2 N3 1.874(7) .
Na1 O1 2.266(7) .
Na1 O1 2.266(7) 20_656
Na1 O1 2.266(7) 26_565
Na1 O1 2.266(7) 11_554
O1 C1 1.205(13) .
N1 N4 1.362(11) .
N1 C1 1.409(12) .
N1 C2 1.383(14) .
N4 N4 1.242(17) 17_665
N2 N3 1.442(11) .
N2 C2 1.283(12) .
N3 C1 1.341(12) .
C2 H2 0.9300 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
Cu1 N2 N3 Cu2 0.000(2) .
Cu1 N2 N3 C1 180.000(2) .
Cu1 N2 C2 N1 180.000(2) .
Cu2 N3 C1 O1 0.000(3) .
Cu2 N3 C1 N1 180.000(2) .
Na1 O1 C1 N1 0.000(3) .
Na1 O1 C1 N3 180.000(2) .
N4 N1 C1 O1 0.000(3) .
N4 N1 C1 N3 180.000(2) .
N4 N1 C2 N2 180.000(2) .
N2 N3 C1 O1 180.000(2) .
N2 N3 C1 N1 0.000(2) .
N3 N2 C2 N1 0.000(2) .
C1 N1 N4 N4 180.000(2) 17_665
C1 N1 C2 N2 0.000(2) .
C2 N1 N4 N4 0.000(3) 17_665
C2 N1 C1 O1 180.000(2) .
C2 N1 C1 N3 0.000(2) .
C2 N2 N3 Cu2 180.000(2) .
C2 N2 N3 C1 0.000(2) .
