#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:41:37 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180273 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/59/7115960.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_7115960
loop_
_publ_author_name
'Ying Xiong'
'Yan-Zhong Fan'
'Rui Yang'
'Sha Chen'
'Mei Pan'
'Ji-Jun Jiang'
'Cheng-Yong Su'
_publ_section_title
;
 Amide and N-oxide functionalization of T-shaped ligands for isoreticular
 MOFs with giant enhancements in CO2 separation
;
_journal_name_full               Chem.Commun.
_journal_page_first              14631
_journal_paper_doi               10.1039/C4cc06697A
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C14 H8 Cu N2 O6'
_chemical_formula_weight         363.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            18
_cell_length_a                   18.569(3)
_cell_length_b                   18.569(3)
_cell_length_c                   40.907(8)
_cell_measurement_reflns_used    3014
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.9574
_cell_measurement_theta_min      2.8863
_cell_volume                     12215(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDE IP'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            37403
_diffrn_reflns_theta_full        89.40
_diffrn_reflns_theta_max         89.40
_diffrn_reflns_theta_min         7.01
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  none
_diffrn_standards_number         3394
_exptl_absorpt_coefficient_mu    1.312
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.400236
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.890
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3294
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    goem
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         6194
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1096
_refine_ls_R_factor_gt           0.0761
_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)+(0.1775P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2375
_refine_ls_wR_factor_ref         0.2652
_reflns_number_gt                3779
_reflns_number_total             6194
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc06697a2.cif
_cod_data_source_block           LIFM-11
_cod_original_cell_volume        12215(3)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7115960
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.52412(3) 0.04827(3) 0.025927(11) 0.0458(3) Uani 1 1 d . . .
O1 O 0.5630(3) 0.1272(2) 0.06738(8) 0.0975(14) Uani 1 1 d D A .
N1 N 0.5466(4) 0.0940(3) 0.09627(11) 0.1032(19) Uani 1 1 d D . .
C1A C 0.4752(12) 0.0867(15) 0.1082(6) 0.129(6) Uani 0.40 1 d PDU A 1
H1A H 0.4505 0.1099 0.0946 0.155 Uiso 0.40 1 calc PR A 1
C2A C 0.4318(12) 0.0507(12) 0.1371(5) 0.117(4) Uani 0.40 1 d PDU A 1
H2A H 0.3765 0.0376 0.1419 0.140 Uiso 0.40 1 calc PR A 1
C3A C 0.4827(16) 0.0377(16) 0.1571(6) 0.106(5) Uani 0.40 1 d PDU A 1
C4A C 0.5392(18) 0.0177(19) 0.1455(7) 0.121(6) Uani 0.40 1 d PDU A 1
H4A H 0.5550 -0.0165 0.1571 0.146 Uiso 0.40 1 calc PR A 1
C5A C 0.5715(19) 0.0516(16) 0.1151(6) 0.139(7) Uani 0.40 1 d PDU A 1
H5A H 0.6153 0.0442 0.1070 0.167 Uiso 0.40 1 calc PR A 1
C6A C 0.4477(14) -0.0109(11) 0.1891(5) 0.194(8) Uani 0.60 1 d PDU A 1
O2A O 0.3674(15) -0.0573(15) 0.1901(6) 0.339(12) Uani 0.60 1 d PDU A 1
C1B C 0.4791(13) 0.0583(12) 0.1130(4) 0.30(2) Uani 0.60 1 d PD A 2
H1B H 0.4300 0.0572 0.1057 0.359 Uiso 0.60 1 calc PR A 2
C2B C 0.4813(11) 0.0207(14) 0.1428(4) 0.157(8) Uani 0.60 1 d PD A 2
H2B H 0.4307 -0.0168 0.1534 0.188 Uiso 0.60 1 calc PR A 2
C3B C 0.5545(11) 0.0373(11) 0.1565(5) 0.133(7) Uani 0.60 1 d PD A 2
C4B C 0.6218(12) 0.0575(14) 0.1387(3) 0.189(8) Uani 0.60 1 d PD A 2
H4B H 0.6685 0.0536 0.1457 0.227 Uiso 0.60 1 calc PR A 2
C5B C 0.6129(11) 0.0851(10) 0.1086(4) 0.163(8) Uani 0.60 1 d PD A 2
H5B H 0.6580 0.1004 0.0939 0.195 Uiso 0.60 1 calc PR A 2
C6B C 0.5466(11) -0.0084(11) 0.1900(4) 0.175(8) Uani 0.40 1 d PDU A 2
O2B O 0.5901(14) -0.0416(16) 0.1933(4) 0.228(8) Uani 0.40 1 d PDU A 2
C7 C 0.4779(3) -0.0444(4) 0.24388(14) 0.0854(17) Uani 1 1 d . A .
C8 C 0.4042(4) -0.0614(4) 0.25924(13) 0.0865(16) Uani 1 1 d . . .
H8A H 0.3662 -0.0493 0.2485 0.104 Uiso 1 1 calc R . .
C9 C 0.3862(3) -0.0967(3) 0.29070(11) 0.0680(12) Uani 1 1 d . . .
C10 C 0.4437(3) -0.1133(3) 0.30653(10) 0.0642(11) Uani 1 1 d . . .
H10A H 0.4326 -0.1353 0.3281 0.077 Uiso 1 1 calc R . .
C11 C 0.5168(3) -0.0975(3) 0.29073(11) 0.0701(12) Uani 1 1 d . . .
C12 C 0.5348(3) -0.0611(4) 0.25930(13) 0.0875(17) Uani 1 1 d . . .
H12A H 0.5855 -0.0481 0.2487 0.105 Uiso 1 1 calc R . .
C13 C 0.3064(3) -0.1191(3) 0.30676(10) 0.0627(11) Uani 1 1 d . . .
C14 C 0.5746(3) -0.1188(3) 0.30687(10) 0.0637(11) Uani 1 1 d . . .
N2 N 0.4957(3) -0.0104(4) 0.21134(12) 0.1007(17) Uani 1 1 d D . .
H13A H 0.5487 0.0149 0.2059 0.121 Uiso 0.50 1 calc PR A 1
H13B H 0.4661 0.0122 0.2052 0.121 Uiso 0.50 1 d PR A 2
O3 O 0.2555(2) -0.1064(2) 0.29088(8) 0.0767(10) Uani 1 1 d . . .
O4 O 0.2963(2) -0.1477(2) 0.33504(7) 0.0722(9) Uani 1 1 d . . .
O5 O 0.6379(2) -0.1071(2) 0.29074(8) 0.0761(9) Uani 1 1 d . . .
O6 O 0.5559(2) -0.1477(2) 0.33493(8) 0.0729(9) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 '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
O5 Cu1 O4 90.39(16) 15_445 8_544
O5 Cu1 O3 88.64(17) 15_445 14
O4 Cu1 O3 168.63(13) 8_544 14
O5 Cu1 O6 168.63(13) 15_445 9_654
O4 Cu1 O6 88.67(15) 8_544 9_654
O3 Cu1 O6 90.05(16) 14 9_654
O5 Cu1 O1 95.51(15) 15_445 .
O4 Cu1 O1 95.33(14) 8_544 .
O3 Cu1 O1 96.04(15) 14 .
O6 Cu1 O1 95.86(14) 9_654 .
O5 Cu1 Cu1 84.72(9) 15_445 10_655
O4 Cu1 Cu1 84.00(9) 8_544 10_655
O3 Cu1 Cu1 84.63(9) 14 10_655
O6 Cu1 Cu1 83.91(9) 9_654 10_655
O1 Cu1 Cu1 179.29(11) . 10_655
N1 O1 Cu1 118.8(3) . .
C1B N1 O1 131.8(12) . .
C1B N1 C5A 85.7(16) . .
O1 N1 C5A 137.5(15) . .
C1B N1 C1A 26.1(17) . .
O1 N1 C1A 111.1(13) . .
C5A N1 C1A 110.0(18) . .
C1B N1 C5B 115.6(13) . .
O1 N1 C5B 111.7(9) . .
C5A N1 C5B 31.7(13) . .
C1A N1 C5B 136.6(15) . .
N1 C1A C2A 131(2) . .
C3A C2A C1A 108(2) . .
C4A C3A C2A 122(3) . .
C4A C3A C6A 107.1(19) . .
C2A C3A C6A 119(2) . .
C5A C4A C3A 114(3) . .
N1 C5A C4A 126(3) . .
O2A C6A N2 124(2) . .
O2A C6A C3A 115(2) . .
N2 C6A C3A 121.1(19) . .
N1 C1B C2B 117(2) . .
C3B C2B C1B 121.1(19) . .
C2B C3B C4B 122.2(19) . .
C2B C3B C6B 115.0(15) . .
C4B C3B C6B 116.7(16) . .
C3B C4B C5B 109.1(18) . .
C4B C5B N1 129.4(17) . .
N2 C6B O2B 124.5(13) . .
N2 C6B C3B 118.6(12) . .
O2B C6B C3B 116.9(14) . .
C12 C7 C8 121.0(5) . .
C12 C7 N2 118.9(5) . .
C8 C7 N2 120.1(5) . .
C7 C8 C9 119.8(5) . .
C10 C9 C8 119.5(5) . .
C10 C9 C13 119.8(4) . .
C8 C9 C13 120.6(4) . .
C11 C10 C9 120.3(4) . .
C10 C11 C12 119.7(4) . .
C10 C11 C14 120.0(4) . .
C12 C11 C14 120.4(4) . .
C7 C12 C11 119.6(5) . .
O4 C13 O3 126.1(4) . .
O4 C13 C9 116.6(4) . .
O3 C13 C9 117.2(4) . .
O6 C14 O5 126.3(4) . .
O6 C14 C11 116.5(4) . .
O5 C14 C11 117.3(4) . .
C6B N2 C6A 91.0(12) . .
C6B N2 C7 130.7(8) . .
C6A N2 C7 130.7(11) . .
C13 O3 Cu1 121.9(3) . 15_445
C13 O4 Cu1 123.0(3) . 6
C14 O5 Cu1 121.8(3) . 14
C14 O6 Cu1 123.1(3) . 5_545
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O5 1.971(3) 15_445
Cu1 O4 1.973(3) 8_544
Cu1 O3 1.975(3) 14
Cu1 O6 1.978(3) 9_654
Cu1 O1 2.119(3) .
Cu1 Cu1 2.6285(10) 10_655
O1 N1 1.297(6) .
N1 C1B 1.282(16) .
N1 C5A 1.340(17) .
N1 C1A 1.353(16) .
N1 C5B 1.416(15) .
C1A C2A 1.399(17) .
C2A C3A 1.359(18) .
C3A C4A 1.362(18) .
C3A C6A 1.54(3) .
C4A C5A 1.384(19) .
C6A O2A 1.297(16) .
C6A N2 1.27(2) .
C1B C2B 1.418(17) .
C2B C3B 1.354(16) .
C3B C4B 1.328(16) .
C3B C6B 1.58(2) .
C4B C5B 1.374(15) .
C6B N2 1.272(16) .
C6B O2B 1.245(15) .
C7 C12 1.392(7) .
C7 C8 1.391(7) .
C7 N2 1.439(7) .
C8 C9 1.406(7) .
C9 C10 1.408(6) .
C9 C13 1.478(6) .
C10 C11 1.396(6) .
C11 C12 1.413(7) .
C11 C14 1.473(6) .
C13 O4 1.247(5) .
C13 O3 1.262(5) .
C14 O6 1.241(5) .
C14 O5 1.267(5) .
O3 Cu1 1.975(3) 15_445
O4 Cu1 1.973(3) 6
O5 Cu1 1.971(3) 14
O6 Cu1 1.978(3) 5_545
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.096 -0.079 -0.001 6812 932 ' '
