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#$Date: 2019-11-10 01:25:07 +0200 (Sun, 10 Nov 2019) $
#$Revision: 225529 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/53/4515376.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_4515376
loop_
_publ_author_name
'Barreda, Omar'
'Bannwart, Gianluca'
'Yap, Glenn P. A.'
'Bloch, Eric D.'
_publ_section_title
;
 Ligand-Based Phase Control in Porous Molecular Assemblies.
;
_journal_issue                   14
_journal_name_full               'ACS applied materials & interfaces'
_journal_page_first              11420
_journal_page_last               11424
_journal_paper_doi               10.1021/acsami.8b02015
_journal_volume                  10
_journal_year                    2018
_chemical_formula_sum            'C22 H20 Cu2 O12'
_chemical_formula_weight         603.46
_space_group_crystal_system      trigonal
_space_group_IT_number           164
_space_group_name_Hall           '-P 3 2"'
_space_group_name_H-M_alt        'P -3 m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   18.6055(11)
_cell_length_b                   18.6055(11)
_cell_length_c                   6.9528(4)
_cell_measurement_reflns_used    5938
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      2.53
_cell_volume                     2084.4(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            13124
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.297
_diffrn_reflns_theta_min         2.189
_exptl_absorpt_coefficient_mu    1.585
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX3 (Bruker, 2015)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       plate
_exptl_crystal_F_000             918
_exptl_crystal_size_max          0.419
_exptl_crystal_size_mid          0.345
_exptl_crystal_size_min          0.206
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         1701
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0348
_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)+(0.0602P)²+1.0901P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.0999
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1441
_reflns_number_total             1701
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            am8b02015_si_008.cif
_cod_data_source_block           eric019_sq
_cod_original_cell_volume        2084.4(3)
_cod_database_code               4515376
_shelx_shelxl_version_number     2017/1
_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. 
;
_shelx_estimated_absorpt_t_min   0.556
_shelx_estimated_absorpt_t_max   0.736
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, 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 0.47604(2) 0.52396(2) 0.65549(5) 0.01946(15) Uani 1 2 d S TU P . .
C1A C 0.07843(16) 0.15764(13) -0.3614(3) 0.124(5) Uani 0.296(3) 1 d DG U P A -1
H1A1 H 0.048252 0.125166 -0.474623 0.186 Uiso 0.296(3) 1 calc R U P A -1
H1A2 H 0.043873 0.174932 -0.291468 0.186 Uiso 0.296(3) 1 calc R U P A -1
H1A3 H 0.091667 0.123618 -0.277182 0.186 Uiso 0.296(3) 1 calc R U P A -1
C2A C 0.15881(15) 0.23444(15) -0.4255(3) 0.062(2) Uani 0.296(3) 1 d DG U P A -1
H2AA H 0.145137 0.265928 -0.519038 0.074 Uiso 0.296(3) 1 calc R U P A -1
H2AB H 0.194116 0.216355 -0.492062 0.074 Uiso 0.296(3) 1 calc R U P A -1
C3A C 0.20820(12) 0.29210(12) -0.2589(2) 0.0457(14) Uani 0.296(3) 1 d DG U P A
-1
H3AA H 0.219604 0.260897 -0.159835 0.055 Uiso 0.296(3) 1 calc R U P A -1
H3AB H 0.261843 0.337887 -0.306310 0.055 Uiso 0.296(3) 1 calc R U P A -1
C1B C 0.08177(16) 0.14459(10) -0.1586(4) 0.124(5) Uani 0.204(3) 1 d DG . P A -2
H1BA H 0.065664 0.114586 -0.036048 0.186 Uiso 0.204(3) 1 calc R U P A -2
H1BB H 0.068151 0.104998 -0.264314 0.186 Uiso 0.204(3) 1 calc R U P A -2
H1BC H 0.051657 0.174850 -0.175770 0.186 Uiso 0.204(3) 1 calc R U P A -2
C2B C 0.17596(15) 0.20653(10) -0.1581(3) 0.062(2) Uani 0.204(3) 1 d DG . P A -2
H2BA H 0.195034 0.222051 -0.023743 0.074 Uiso 0.204(3) 1 calc R U P A -2
H2BB H 0.205282 0.179241 -0.213385 0.074 Uiso 0.204(3) 1 calc R U P A -2
C3B C 0.19871(12) 0.28520(12) -0.2733(2) 0.0457(14) Uani 0.204(3) 1 d DG . P A
-2
H3BA H 0.259669 0.322219 -0.276325 0.055 Uiso 0.204(3) 1 calc R U P A -2
H3BB H 0.178286 0.270882 -0.407180 0.055 Uiso 0.204(3) 1 calc R U P A -2
C4 C 0.18163(8) 0.36325(9) -0.00984(18) 0.0317(7) Uani 1 2 d G T P A .
C5 C 0.25742(7) 0.38496(6) 0.07674(13) 0.0290(5) Uani 1 1 d G . . . .
H5 H 0.295877 0.373448 0.013837 0.035 Uiso 1 1 calc R U . . .
C6 C 0.27649(5) 0.42371(6) 0.25631(12) 0.0245(5) Uani 1 1 d G . . . .
C7 C 0.22089(7) 0.44179(11) 0.34842(18) 0.0253(6) Uani 1 2 d G T P . .
H7 H 0.233098 0.466196 0.472791 0.030 Uiso 1 2 calc R U P . .
C8 C 0.35925(5) 0.44995(6) 0.34799(12) 0.0234(4) Uani 1 1 d G . . . .
O1 O 0.16162(10) 0.32324(11) -0.18243(19) 0.0484(7) Uani 1 2 d G TU P . .
O2 O 0.37090(7) 0.48011(7) 0.51341(12) 0.0366(4) Uani 1 1 d G U . . .
O3 O 0.41075(6) 0.44038(10) 0.25090(16) 0.0342(4) Uani 1 1 d G . . . .
O4 O 0.43685(12) 0.56316(14) 0.90402(19) 0.0458(7) Uani 1 2 d G 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'
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
O2 Cu1 O2 89.55(9) . 10_665
O2 Cu1 O3 167.6 . 7_666
O2 Cu1 O3 89.38(14) 10_665 7_666
O2 Cu1 O3 89.38(8) . 4_556
O2 Cu1 O3 167.57(9) 10_665 4_556
O3 Cu1 O3 89.01(14) 7_666 4_556
O2 Cu1 O4 96.26(6) . .
O2 Cu1 O4 96.26(6) 10_665 .
O3 Cu1 O4 96.16(9) 7_666 .
O3 Cu1 O4 96.16(10) 4_556 .
O2 Cu1 Cu1 83.29(3) . 7_666
O2 Cu1 Cu1 83.29(7) 10_665 7_666
O3 Cu1 Cu1 84.29(6) 7_666 7_666
O3 Cu1 Cu1 84.29(6) 4_556 7_666
O4 Cu1 Cu1 179.36(5) . 7_666
C2A C1A H1A1 109.5 . .
C2A C1A H1A2 109.5 . .
H1A1 C1A H1A2 109.5 . .
C2A C1A H1A3 109.5 . .
H1A1 C1A H1A3 109.5 . .
H1A2 C1A H1A3 109.5 . .
C1A C2A C3A 113.4 . .
C1A C2A H2AA 108.9 . .
C3A C2A H2AA 108.9 . .
C1A C2A H2AB 108.9 . .
C3A C2A H2AB 108.9 . .
H2AA C2A H2AB 107.7 . .
O1 C3A C2A 107.8 . .
O1 C3A H3AA 110.2 . .
C2A C3A H3AA 110.2 . .
O1 C3A H3AB 110.2 . .
C2A C3A H3AB 110.2 . .
H3AA C3A H3AB 108.5 . .
C2B C1B H1BA 109.5 . .
C2B C1B H1BB 109.5 . .
H1BA C1B H1BB 109.5 . .
C2B C1B H1BC 109.5 . .
H1BA C1B H1BC 109.5 . .
H1BB C1B H1BC 109.5 . .
C3B C2B C1B 112.4 . .
C3B C2B H2BA 109.1 . .
C1B C2B H2BA 109.1 . .
C3B C2B H2BB 109.1 . .
C1B C2B H2BB 109.1 . .
H2BA C2B H2BB 107.9 . .
O1 C3B C2B 106.5 . .
O1 C3B H3BA 110.4 . .
C2B C3B H3BA 110.4 . .
O1 C3B H3BB 110.4 . .
C2B C3B H3BB 110.4 . .
H3BA C3B H3BB 108.6 . .
O1 C4 C5 119.9 . .
O1 C4 C5 119.9 . 11
C5 C4 C5 120.1 . 11
C4 C5 C6 119.7 . .
C4 C5 H5 120.2 . .
C6 C5 H5 120.2 . .
C7 C6 C5 120.5 . .
C7 C6 C8 119.3 . .
C5 C6 C8 120.1 . .
C6 C7 C6 119.3 11 .
C6 C7 H7 120.3 11 .
C6 C7 H7 120.3 . .
O2 C8 O3 125.8 . .
O2 C8 C6 117.1 . .
O3 C8 C6 117.1 . .
C4 O1 C3B 128.3 . .
C4 O1 C3A 121.1 . .
C8 O2 Cu1 124.1 . .
C8 O3 Cu1 122.4 . 7_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O2 1.9678 .
Cu1 O2 1.9678(13) 10_665
Cu1 O3 1.9756(10) 7_666
Cu1 O3 1.9756(17) 4_556
Cu1 O4 2.1405(14) .
Cu1 Cu1 2.6569(7) 7_666
C1A C2A 1.5296 .
C1A H1A1 0.9800 .
C1A H1A2 0.9800 .
C1A H1A3 0.9800 .
C2A C3A 1.5331 .
C2A H2AA 0.9900 .
C2A H2AB 0.9900 .
C3A O1 1.3680 .
C3A H3AA 0.9900 .
C3A H3AB 0.9900 .
C1B C2B 1.5425 .
C1B H1BA 0.9800 .
C1B H1BB 0.9800 .
C1B H1BC 0.9800 .
C2B C3B 1.5308 .
C2B H2BA 0.9900 .
C2B H2BB 0.9900 .
C3B O1 1.3655 .
C3B H3BA 0.9900 .
C3B H3BB 0.9900 .
C4 O1 1.3622 .
C4 C5 1.3944 .
C4 C5 1.3945(19) 11
C5 C6 1.3959 .
C5 H5 0.9500 .
C6 C7 1.3933 .
C6 C8 1.5045 .
C7 H7 0.9500 .
C8 O2 1.2502 .
C8 O3 1.2554 .
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
C1A C2A C3A O1 -65.0 . .
C1B C2B C3B O1 63.2 . .
O1 C4 C5 C6 -178.1 . .
C5 C4 C5 C6 4.1 11 .
C4 C5 C6 C7 -0.8 . .
C4 C5 C6 C8 -178.0 . .
C5 C6 C7 C6 -2.4 . 11
C8 C6 C7 C6 174.7 . 11
C7 C6 C8 O2 6.7 . .
C5 C6 C8 O2 -176.1 . .
C7 C6 C8 O3 -172.6 . .
C5 C6 C8 O3 4.6 . .
C5 C4 O1 C3B 14.1 . .
C5 C4 O1 C3B -168.1 11 .
C5 C4 O1 C3A 10.4 . .
C5 C4 O1 C3A -171.8 11 .
C2B C3B O1 C4 71.0 . .
C2A C3A O1 C4 167.0 . .
O3 C8 O2 Cu1 2.60(7) . .
C6 C8 O2 Cu1 -176.65(7) . .
O2 C8 O3 Cu1 -2.03(10) . 7_666
C6 C8 O3 Cu1 177.23(10) . 7_666
