#------------------------------------------------------------------------------
#$Date: 2017-09-06 14:00:00 +0300 (Wed, 06 Sep 2017) $
#$Revision: 200217 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/41/4514177.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_4514177
loop_
_publ_author_name
'Chen, Ya'
'Wang, Bin'
'Wang, Xiaoqing'
'Xie, Lin-Hua'
'Li, Jinping'
'Xie, Yabo'
'Li, Jian-Rong'
_publ_section_title
;
 A Copper(II)-Paddlewheel Metal-Organic Framework with Exceptional
 Hydrolytic Stability and Selective Adsorption and Detection Ability of
 Aniline in Water.
;
_journal_issue                   32
_journal_name_full               'ACS applied materials & interfaces'
_journal_page_first              27027
_journal_page_last               27035
_journal_paper_doi               10.1021/acsami.7b07920
_journal_volume                  9
_journal_year                    2017
_chemical_formula_moiety         'C100 H60 Cu8 O40, 46.48(O)'
_chemical_formula_sum            'C100 H168.96 Cu8 O86.48'
_chemical_formula_weight         3263.30
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           129
_space_group_name_Hall           '-P 4a 2a'
_space_group_name_H-M_alt        'P 4/n m m'
_symmetry_space_group_name_Hall  '-P 4a 2a'
_symmetry_space_group_name_H-M   'P 4/n m m :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-05-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   18.9911(10)
_cell_length_b                   18.9911(10)
_cell_length_c                   13.4276(13)
_cell_measurement_reflns_used    2543
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      67.2050
_cell_measurement_theta_min      4.6260
_cell_volume                     4842.8(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -114.00  -14.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8105  -57.0000  150.0000 100

#__ type_ start__ end____ width___ exp.time_
  2 omega  -49.00   33.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8105   37.0000  120.0000 82

#__ type_ start__ end____ width___ exp.time_
  3 omega  -96.00   -2.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8105  125.0000   30.0000 94

#__ type_ start__ end____ width___ exp.time_
  4 omega   30.00   90.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  -30.0000   60.0000 60

#__ type_ start__ end____ width___ exp.time_
  5 omega   78.00  178.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759   30.0000 -120.0000 100

#__ type_ start__ end____ width___ exp.time_
  6 omega   23.00  109.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  -94.0000  -60.0000 86

#__ type_ start__ end____ width___ exp.time_
  7 omega   78.00  178.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759   30.0000  -30.0000 100

#__ type_ start__ end____ width___ exp.time_
  8 omega   33.00   98.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  -45.0000 -180.0000 65

#__ type_ start__ end____ width___ exp.time_
  9 omega   33.00   98.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  -45.0000  -90.0000 65

#__ type_ start__ end____ width___ exp.time_
 10 omega   23.00  109.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  -94.0000   30.0000 86

#__ type_ start__ end____ width___ exp.time_
 11 omega -114.00  -20.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8105  -57.0000   30.0000 94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1522
_diffrn_reflns_av_unetI/netI     0.0640
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27132
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.233
_diffrn_reflns_theta_min         4.032
_exptl_absorpt_coefficient_mu    1.634
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description       block
_exptl_crystal_F_000             1693
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1392
_refine_ls_R_factor_gt           0.0903
_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)+(0.1913P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2557
_refine_ls_wR_factor_ref         0.2974
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1583
_reflns_number_total             2724
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            am7b07920_si_002.cif
_cod_data_source_block           water@BUT-155
_cod_original_cell_volume        4842.8(7)
_cod_database_code               4514177
_shelxl_version_number           2014-1
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H8A(0.25) H8B(0.25) H8C(0.25) H11B(0.5) H11C(0.5) O5(0.75) O6(0.3)
 O4(0.3) O8(0.105) O12(0.5) O10(0.3) O9(0.25) O7(0.25) O11(0.15)
3.a Me refined with riding coordinates:
 C8(H8A,H8B,H8C), C11(H11A,H11B,H11C)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3)
;
_olex2_date_sample_data_collection 2016-07-24
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/2, x, z'
'-x+1/2, -y+1/2, z'
'y, -x+1/2, z'
'x+1/2, -y, -z'
'-x, y+1/2, -z'
'y+1/2, x+1/2, -z'
'-y, -x, -z'
'-x, -y, -z'
'y-1/2, -x, -z'
'x-1/2, y-1/2, -z'
'-y, x-1/2, -z'
'-x-1/2, y, z'
'x, -y-1/2, z'
'-y-1/2, -x-1/2, z'
'y, x, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.46725(4) 0.46725(4) 0.57279(9) 0.0376(4) Uani 1 2 d S T P . .
O2 O 0.3798(2) 0.4825(2) 0.4984(4) 0.0530(12) Uani 1 1 d . . . . .
O1 O 0.4603(2) 0.5634(2) 0.6229(3) 0.0520(11) Uani 1 1 d . . . . .
O3 O 0.4166(3) 0.4166(3) 0.6986(5) 0.0627(19) Uani 1 2 d S T P . .
C9 C 0.2500 0.6856(5) 0.1063(6) 0.0400(18) Uani 1 2 d S T P . .
C6 C 0.2500 0.6863(4) 0.2106(6) 0.0368(17) Uani 1 2 d S T P . .
C10 C 0.2500 0.7500 0.0535(8) 0.039(2) Uani 1 4 d S T P . .
C4 C 0.3129(3) 0.5930(3) 0.3034(4) 0.0425(13) Uani 1 1 d . . . . .
H4 H 0.3562 0.6102 0.2777 0.051 Uiso 1 1 calc R . . . .
C3 C 0.2500 0.5134(5) 0.4123(6) 0.0430(19) Uani 1 2 d S T P . .
H3 H 0.2500 0.4782 0.4625 0.052 Uiso 1 2 calc RS T P . .
C5 C 0.2500 0.6208(4) 0.2698(6) 0.0398(18) Uani 1 2 d S T P . .
C7 C 0.2500 0.7500 0.2618(8) 0.041(3) Uani 1 4 d S T P . .
C8 C 0.2500 0.7500 0.3758(8) 0.051(3) Uani 1 4 d S T P . .
H8A H 0.2500 0.7013 0.4002 0.076 Uiso 0.5 2 calc RS T P . .
H8B H 0.2079 0.7743 0.4002 0.076 Uiso 0.25 1 calc R . . . .
H8C H 0.2921 0.7743 0.4002 0.076 Uiso 0.25 1 calc R . . . .
C2 C 0.3132(3) 0.5392(3) 0.3755(5) 0.0420(13) Uani 1 1 d . . . . .
C11 C 0.2500 0.6171(5) 0.0485(7) 0.054(2) Uani 1 2 d S T P . .
H11A H 0.2500 0.6272 -0.0230 0.081 Uiso 1 2 calc RS T P . .
H11B H 0.2079 0.5899 0.0656 0.081 Uiso 0.5 1 calc R . . . .
H11C H 0.2921 0.5899 0.0656 0.081 Uiso 0.5 1 calc R . . . .
C1 C 0.3825(3) 0.5186(3) 0.4194(5) 0.0452(13) Uani 1 1 d . . . . .
O5_a O 0.5133(7) 0.3507(12) 0.8239(13) 0.237(11) Uani 0.75 1 d . . . A 1
O6_b O 0.3231(6) 0.3231(6) 0.616(2) 0.167(11) Uani 0.6 2 d S T P B 2
O4_c O 0.1746(8) 0.3254(8) 0.3983(19) 0.146(8) Uani 0.6 2 d S T P C 3
O8_d O 0.549(2) 0.2500 0.671(3) 0.18(4) Uani 0.21 2 d S T P D 4
O12_e O 0.0768(12) 0.5324(19) 0.110(2) 0.237(18) Uani 0.5 1 d . . . E 5
O10_f O 0.173(2) 0.408(2) 0.179(4) 0.31(4) Uani 0.3 1 d . . . F 6
O9_g O 0.4341(15) 0.2500 0.9312(18) 0.176(15) Uani 0.5 2 d S T P G 7
O7_h O 0.5741(16) 0.2500 0.771(3) 0.181(14) Uani 0.5 2 d S T P H 8
O11_i O 0.0379(16) 0.4621(16) 0.173(3) 0.20(4) Uani 0.3 2 d S T P I 9
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'
Cu Cu -1.9646 0.5888 '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'
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 Cu1 87.24(13) . 9_666
O2 Cu1 Cu1 87.24(13) 16 9_666
O2 Cu1 O2 89.5(3) 16 .
O2 Cu1 O3 95.0(2) . .
O2 Cu1 O3 95.0(2) 16 .
O1 Cu1 Cu1 81.13(13) 16 9_666
O1 Cu1 Cu1 81.13(13) . 9_666
O1 Cu1 O2 88.9(2) 16 16
O1 Cu1 O2 88.9(2) . .
O1 Cu1 O2 168.32(19) . 16
O1 Cu1 O2 168.32(19) 16 .
O1 Cu1 O1 90.4(3) . 16
O1 Cu1 O3 96.7(2) . .
O1 Cu1 O3 96.7(2) 16 .
O3 Cu1 Cu1 176.9(2) . 9_666
C1 O2 Cu1 118.3(4) . .
C1 O1 Cu1 126.5(4) 8_666 .
C6 C9 C10 119.6(8) . .
C6 C9 C11 121.3(8) . .
C10 C9 C11 119.1(8) . .
C9 C6 C5 122.1(8) . .
C7 C6 C9 120.1(8) . .
C7 C6 C5 117.8(7) . .
C9 C10 C9 119.8(10) 3_565 .
C9 C10 C10 120.1(5) 3_565 10_565
C9 C10 C10 120.1(5) . 10_565
C5 C4 H4 119.8 . .
C5 C4 C2 120.4(6) . .
C2 C4 H4 119.8 . .
C2 C3 H3 120.1 . .
C2 C3 H3 120.1 13_655 .
C2 C3 C2 119.8(8) 13_655 .
C4 C5 C6 119.9(4) 13_655 .
C4 C5 C6 119.9(4) . .
C4 C5 C4 119.6(8) . 13_655
C6 C7 C6 120.8(10) . 3_565
C6 C7 C8 119.6(5) . .
C6 C7 C8 119.6(5) 3_565 .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8B 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C4 C2 C1 117.8(5) . .
C3 C2 C4 119.8(6) . .
C3 C2 C1 121.9(6) . .
C9 C11 H11A 109.5 . .
C9 C11 H11B 109.5 . .
C9 C11 H11C 109.5 . .
H11A C11 H11B 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
O2 C1 C2 116.0(6) . .
O1 C1 O2 126.4(6) 8_666 .
O1 C1 C2 117.6(6) 8_666 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 Cu1 2.630(2) 9_666
Cu1 O2 1.960(4) .
Cu1 O2 1.960(4) 16
Cu1 O1 1.950(4) 16
Cu1 O1 1.950(4) .
Cu1 O3 2.169(6) .
O2 C1 1.263(7) .
O1 C1 1.242(8) 8_666
C9 C6 1.400(11) .
C9 C10 1.414(10) .
C9 C11 1.515(12) .
C6 C5 1.475(11) .
C6 C7 1.392(9) .
C10 C9 1.414(10) 3_565
C10 C10 1.44(2) 10_565
C4 H4 0.9500 .
C4 C5 1.382(7) .
C4 C2 1.406(8) .
C3 H3 0.9500 .
C3 C2 1.388(7) .
C3 C2 1.388(7) 13_655
C5 C4 1.382(7) 13_655
C7 C6 1.392(9) 3_565
C7 C8 1.531(15) .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C2 C1 1.493(8) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C1 O1 1.242(8) 8_666
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_1
_geom_torsion_site_symmetry_4
Cu1 O2 C1 O1 8.4(9) . 8_666
Cu1 O2 C1 C2 -169.6(4) . .
C9 C6 C5 C4 -94.6(7) . 13_655
C9 C6 C5 C4 94.6(7) . .
C9 C6 C7 C6 0.000(2) . 3_565
C9 C6 C7 C8 180.000(3) . .
C6 C9 C10 C9 0.000(4) . 3_565
C6 C9 C10 C10 180.000(3) . 10_565
C10 C9 C6 C5 180.000(3) . .
C10 C9 C6 C7 0.000(3) . .
C4 C2 C1 O2 164.5(6) . .
C4 C2 C1 O1 -13.6(9) . 8_666
C3 C2 C1 O2 -7.4(10) . .
C3 C2 C1 O1 174.4(7) . 8_666
C5 C6 C7 C6 180.000(0) . 3_565
C5 C6 C7 C8 0.000(3) . .
C5 C4 C2 C3 0.7(11) . .
C5 C4 C2 C1 -171.4(6) . .
C7 C6 C5 C4 85.4(7) . 13_655
C7 C6 C5 C4 -85.4(7) . .
C2 C4 C5 C6 167.4(7) . .
C2 C4 C5 C4 -3.5(13) . 13_655
C2 C3 C2 C4 2.0(13) 13_655 .
C2 C3 C2 C1 173.8(5) 13_655 .
C11 C9 C6 C5 0.000(3) . .
C11 C9 C6 C7 180.000(3) . .
C11 C9 C10 C9 180.000(2) . 3_565
C11 C9 C10 C10 0.000(4) . 10_565
