#------------------------------------------------------------------------------
#$Date: 2016-03-26 12:50:16 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180216 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/02/7110280.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_7110280
loop_
_publ_author_name
'Dybtsev, Danil N.'
'Chun, Hyungphil'
'Kim, Kimoon'
_publ_section_title
;
 Three-dimensional metal?organic framework with (3,4)-connected net,
 synthesized from an ionic liquid mediumElectronic supplementary
 information (ESI) available: IR, XRD, TGA, details of data collection and
 structure refinements, as well as additional figures related to the
 framework. See http://www.rsc.org/suppdata/cc/b4/b403001j/
;
_journal_issue                   14
_journal_name_full               'Chemical Communications'
_journal_page_first              1594
_journal_page_last               1595
_journal_paper_doi               10.1039/b403001j
_journal_year                    2004
_chemical_formula_sum            'C84 H66 B3 Cu3 F12 N28 O5'
_chemical_formula_weight         1998.70
_chemical_name_systematic
;
?
;
_space_group_IT_number           230
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-I 4bd 2c 3'
_symmetry_space_group_name_H-M   'I a -3 d'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.019(3)
_cell_length_b                   28.019(3)
_cell_length_c                   28.019(3)
_cell_measurement_temperature    223(2)
_cell_volume                     21997(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Diamond
_computing_publication_material  'MS WORD'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR2002
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SMART CCD'
_diffrn_measurement_method       'omega scan'
_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  0.0600
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            54682
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_T_max  0.7808
_exptl_absorpt_correction_T_min  0.7367
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            'dark violet'
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rhombic dodecahedral'
_exptl_crystal_F_000             8128
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.126
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         1814
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0966
_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)+(0.1896P)²+76.5332P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2772
_refine_ls_wR_factor_ref         0.2993
_reflns_number_gt                1486
_reflns_number_total             1814
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b403001jsup1.cif
_cod_data_source_block           1
_cod_original_cell_volume        21996(4)
_cod_database_code               7110280
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+3/4, x+1/4, -z+1/4'
'-y+3/4, -x+3/4, -z+3/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/4'
'-x+1/4, z+3/4, y+1/4'
'-x+3/4, -z+3/4, -y+3/4'
'x+1/4, -z+1/4, y+3/4'
'z+3/4, y+1/4, -x+1/4'
'z+1/4, -y+1/4, x+3/4'
'-z+1/4, y+3/4, x+1/4'
'-z+3/4, -y+3/4, -x+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'y+5/4, x+3/4, -z+3/4'
'-y+5/4, -x+5/4, -z+5/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'x+5/4, z+3/4, -y+3/4'
'-x+3/4, z+5/4, y+3/4'
'-x+5/4, -z+5/4, -y+5/4'
'x+3/4, -z+3/4, y+5/4'
'z+5/4, y+3/4, -x+3/4'
'z+3/4, -y+3/4, x+5/4'
'-z+3/4, y+5/4, x+3/4'
'-z+5/4, -y+5/4, -x+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-1/2'
'-y-3/4, -x-1/4, z-1/4'
'y-3/4, x-3/4, z-3/4'
'-y-1/4, x-1/4, -z-3/4'
'y-1/4, -x-3/4, -z-1/4'
'-x-3/4, -z-1/4, y-1/4'
'x-1/4, -z-3/4, -y-1/4'
'x-3/4, z-3/4, y-3/4'
'-x-1/4, z-1/4, -y-3/4'
'-z-3/4, -y-1/4, x-1/4'
'-z-1/4, y-1/4, -x-3/4'
'z-1/4, -y-3/4, -x-1/4'
'z-3/4, y-3/4, x-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'x+1/2, -y, z'
'-x, y, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z, x, y+1/2'
'z, x+1/2, -y'
'z+1/2, -x, y'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z, x'
'-y, z, x+1/2'
'y, z+1/2, -x'
'-y-1/4, -x+1/4, z+1/4'
'y-1/4, x-1/4, z-1/4'
'-y+1/4, x+1/4, -z-1/4'
'y+1/4, -x-1/4, -z+1/4'
'-x-1/4, -z+1/4, y+1/4'
'x+1/4, -z-1/4, -y+1/4'
'x-1/4, z-1/4, y-1/4'
'-x+1/4, z+1/4, -y-1/4'
'-z-1/4, -y+1/4, x+1/4'
'-z+1/4, y+1/4, -x-1/4'
'z+1/4, -y-1/4, -x+1/4'
'z-1/4, y-1/4, x-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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.3750 0.0000 0.2500 0.0346(5) Uani 1 4 d S . .
N1 N 0.33411(16) 0.05892(16) 0.24202(15) 0.0504(11) Uani 1 1 d . . .
N2 N 0.2033(5) 0.1804(5) 0.2485(6) 0.066(4) Uani 0.62(3) 1 d PU A 1
C1 C 0.2905(5) 0.0601(5) 0.2645(5) 0.047(3) Uani 0.62(3) 1 d PU A 1
H1A H 0.2814 0.0345 0.2842 0.056 Uiso 0.62(3) 1 calc PR A 1
C2 C 0.2598(7) 0.0982(7) 0.2587(7) 0.060(4) Uani 0.62(3) 1 d PU A 1
H2A H 0.2322 0.1004 0.2775 0.072 Uiso 0.62(3) 1 calc PR A 1
C3 C 0.2698(5) 0.1329(5) 0.2254(5) 0.049(3) Uani 0.62(3) 1 d PU A 1
C4 C 0.3120(6) 0.1272(5) 0.1983(6) 0.055(3) Uani 0.62(3) 1 d PU A 1
H4A H 0.3203 0.1494 0.1745 0.066 Uiso 0.62(3) 1 calc PR A 1
C5 C 0.3400(7) 0.0894(7) 0.2071(7) 0.048(4) Uani 0.62(3) 1 d PU A 1
H5A H 0.3661 0.0843 0.1866 0.057 Uiso 0.62(3) 1 calc PR A 1
C6 C 0.2385(6) 0.1742(6) 0.2183(6) 0.063(4) Uani 0.62(3) 1 d PU A 1
N2' N 0.2207(10) 0.1971(9) 0.2643(9) 0.070(6) Uani 0.38(3) 1 d PU A 2
C1' C 0.3000(7) 0.0715(7) 0.2730(7) 0.034(4) Uiso 0.38(3) 1 d PU A 2
H1'A H 0.2947 0.0512 0.2992 0.041 Uiso 0.38(3) 1 calc PR A 2
C2' C 0.2720(9) 0.1115(9) 0.2697(9) 0.042(4) Uani 0.38(3) 1 d PU A 2
H2'A H 0.2445 0.1144 0.2887 0.050 Uiso 0.38(3) 1 calc PR A 2
C3' C 0.2845(8) 0.1472(9) 0.2387(8) 0.048(5) Uani 0.38(3) 1 d PU A 2
C4' C 0.3260(10) 0.1421(9) 0.2129(10) 0.058(5) Uani 0.38(3) 1 d PU A 2
H4'A H 0.3367 0.1663 0.1922 0.070 Uiso 0.38(3) 1 calc PR A 2
C5' C 0.3517(10) 0.0996(12) 0.2184(11) 0.044(5) Uani 0.38(3) 1 d PU A 2
H5'A H 0.3826 0.0982 0.2056 0.053 Uiso 0.38(3) 1 calc PR A 2
C6' C 0.2560(9) 0.1903(10) 0.2353(11) 0.064(6) Uani 0.38(3) 1 d PU A 2
N1S N 0.1813(7) -0.1770(7) 0.3803(7) 0.026(4) Uiso 0.17 1 d P B 1
C1S C 0.1979(7) -0.1388(7) 0.3577(7) 0.022(4) Uiso 0.17 1 d P B 1
C2S C 0.2430(4) -0.1163(3) 0.3759(5) 0.027(5) Uiso 0.17 1 d PG B 1
C3S C 0.2572(3) -0.0724(3) 0.3577(3) 0.028(5) Uiso 0.17 1 d PG B 1
C4S C 0.2990(3) -0.0511(4) 0.3740(4) 0.053(8) Uiso 0.17 1 d PG B 1
N2S N 0.3265(4) -0.0738(5) 0.4084(5) 0.046(5) Uiso 0.17 1 d PG B 1
C6S C 0.3124(5) -0.1177(5) 0.4266(5) 0.047(7) Uiso 0.17 1 d PG B 1
C5S C 0.2706(5) -0.1390(4) 0.4103(5) 0.041(6) Uiso 0.17 1 d PG B 1
B1 B 0.2484(4) -0.0016(3) 0.3750(4) 0.6(3) Uiso 0.50 2 d SPG B 2
F1 F 0.2240(4) -0.0059(4) 0.3308(4) 0.230(9) Uiso 0.50 1 d PG B 2
F2 F 0.2452(6) 0.0465(3) 0.3752(6) 0.228(10) Uiso 0.50 1 d PG B 2
O1W O 0.1501(4) -0.1249(7) 0.4001(10) 0.060 Uiso 0.148(15) 2 d SPG B 2
O2W O 0.2443(4) -0.0315(3) 0.3406(3) 0.060 Uiso 0.241(10) 1 d PG B 3
O3W O 0.2781(6) 0.0281(3) 0.3750(6) 0.060 Uiso 0.203(14) 2 d SPG B 3
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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'
Cu Cu 0.3201 1.2651 '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
N1 Cu1 N1 111.0(3) 28_445 .
N1 Cu1 N1 108.73(13) 28_445 89_655
N1 Cu1 N1 108.73(13) . 89_655
N1 Cu1 N1 108.73(13) 28_445 68_656
N1 Cu1 N1 108.73(13) . 68_656
N1 Cu1 N1 111.0(3) 89_655 68_656
C5 N1 C1' 113.8(12) . .
C5 N1 C1 116.1(10) . .
C1' N1 C1 20.2(8) . .
C5 N1 C5' 22.4(10) . .
C1' N1 C5' 110.0(16) . .
C1 N1 C5' 120.4(14) . .
C5 N1 Cu1 122.9(9) . .
C1' N1 Cu1 123.2(9) . .
C1 N1 Cu1 118.2(6) . .
C5' N1 Cu1 121.0(13) . .
C6 N2 C6 114.7(12) . 9
N1 C1 C2 121.2(11) . .
C3 C2 C1 120.0(15) . .
C2 C3 C4 117.0(13) . .
C2 C3 C6 121.8(13) . .
C4 C3 C6 121.2(11) . .
C5 C4 C3 118.7(14) . .
N1 C5 C4 125.4(17) . .
N2 C6 N2 125.2(12) . 5
N2 C6 C3 117.9(10) . .
N2 C6 C3 116.9(10) 5 .
C6' N2' C6' 118(2) . 9
N1 C1' C2' 125.4(18) . .
C1' C2' C3' 120(2) . .
C2' C3' C4' 118(2) . .
C2' C3' C6' 121(2) . .
C4' C3' C6' 121.0(18) . .
C3' C4' C5' 118(2) . .
C4' C5' N1 124(2) . .
N2' C6' N2' 122(2) . 5
N2' C6' C3' 120(2) . .
N2' C6' C3' 118.0(19) 5 .
C1S N1S C1S 116(2) . 7
N1S C1S N1S 124(2) . 10_545
N1S C1S C2S 118.2(17) . .
N1S C1S C2S 118.2(17) 10_545 .
C3S C2S C5S 120.0 . .
C3S C2S C1S 119.2(10) . .
C5S C2S C1S 120.8(10) . .
C4S C3S C2S 120.0 . .
C3S C4S N2S 120.0 . .
C6S N2S C4S 120.0 . .
C6S N2S C6S 14.4(7) . 24_545
C4S N2S C6S 133.7(9) . 24_545
C6S C6S N2S 130(3) 24_545 .
C6S C6S C5S 108(3) 24_545 .
N2S C6S C5S 120.0 . .
C6S C6S C5S 52(2) 24_545 24_545
N2S C6S C5S 95.4(12) . 24_545
C5S C6S C5S 136.2(7) . 24_545
C6S C6S N2S 35.3(17) 24_545 24_545
N2S C6S N2S 130.3(5) . 24_545
C5S C6S N2S 88.6(12) . 24_545
C5S C6S N2S 86.5(9) 24_545 24_545
C6S C5S C2S 120.0 . .
C6S C5S C6S 19.9(8) . 24_545
C2S C5S C6S 139.2(7) . 24_545
F2 B1 F2 97.5(7) . 37_445
F2 B1 F1 118.0(6) . 37_445
F2 B1 F1 93.2(14) 37_445 37_445
F2 B1 F1 93.2 . .
F2 B1 F1 118.1(12) 37_445 .
F1 B1 F1 132.9(4) 37_445 .
O1W O1W O1W 60.0 7 10_545
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 2.022(4) 28_445
Cu1 N1 2.022(4) .
Cu1 N1 2.022(4) 89_655
Cu1 N1 2.022(4) 68_656
N1 C5 1.31(2) .
N1 C1' 1.34(2) .
N1 C1 1.375(12) .
N1 C5' 1.41(3) .
N2 C6 1.312(17) .
N2 C6 1.367(16) 9
C1 C2 1.38(2) .
C2 C3 1.38(2) .
C3 C4 1.414(18) .
C3 C6 1.466(17) .
C4 C5 1.34(2) .
C6 N2 1.367(16) 5
N2' C6' 1.29(3) .
N2' C6' 1.39(3) 9
C1' C2' 1.37(3) .
C2' C3' 1.37(3) .
C3' C4' 1.38(3) .
C3' C6' 1.45(3) .
C4' C5' 1.40(4) .
C6' N2' 1.39(3) 5
N1S C1S 1.33(3) .
N1S C1S 1.35(3) 7
C1S N1S 1.35(3) 10_545
C1S C2S 1.50(2) .
C2S C3S 1.3900 .
C2S C5S 1.3900 .
C3S C4S 1.3900 .
C4S N2S 1.3900 .
N2S C6S 1.3900 .
N2S C6S 1.83(2) 24_545
C6S C6S 0.598(18) 24_545
C6S C5S 1.3900 .
C6S C5S 1.67(2) 24_545
C6S N2S 1.83(2) 24_545
C5S C6S 1.67(3) 24_545
B1 F2 1.3525 .
B1 F2 1.352(19) 37_445
B1 F1 1.42(2) 37_445
B1 F1 1.4184 .
O1W O1W 1.72(4) 7
O1W O1W 1.72(3) 10_545
