#------------------------------------------------------------------------------
#$Date: 2020-05-21 01:06:02 +0300 (Thu, 21 May 2020) $
#$Revision: 252213 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/35/4003543.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_4003543
loop_
_publ_author_name
'Krause, Simon'
'Reuter, Florian S.'
'Ehrling, Sebastian'
'Bon, Volodymyr'
'Senkovska, Irena'
'Kaskel, Stefan'
'Brunner, Eike'
_publ_section_title
;
 Impact of Defects and Crystal Size on Negative Gas Adsorption in DUT-49
 Analyzed by In Situ 129Xe NMR Spectroscopy
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.0c01059
_journal_year                    2020
_chemical_formula_sum            'C32 H26 Cu2 N2 O10'
_chemical_formula_weight         725.63
_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-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   23.515(3)
_cell_length_b                   23.515(3)
_cell_length_c                   11.052(2)
_cell_measurement_reflns_used    573
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.83
_cell_measurement_theta_min      3.85
_cell_volume                     5292.5(14)
_computing_cell_refinement       'XDSAPP 2.0 Sparta et al., 2016'
_computing_data_collection       'marCCD 1994-2002'
_computing_data_reduction        'XDSAPP 2.0 Sparta et al., 2016'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'MX-225 CCD'
_diffrn_measurement_method       'Δφ scans'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.88561
_diffrn_reflns_av_R_equivalents  0.0854
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            41015
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        32.098
_diffrn_reflns_theta_max         35.098
_diffrn_reflns_theta_min         1.246
_diffrn_source                   synchrotron
_diffrn_source_type              'BESSY BL MX-14.2'
_exptl_absorpt_coefficient_mu    1.139
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.683
_exptl_crystal_description       block
_exptl_crystal_F_000             1110
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.287
_refine_diff_density_min         -1.551
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.273
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         4222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.273
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_gt           0.1039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2500P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3214
_refine_ls_wR_factor_ref         0.3435
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3530
_reflns_number_total             4222
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm0c01059_si_002.cif
_cod_data_source_block           p3m1_sq
_cod_original_cell_volume        5292.5(18)
_cod_database_code               4003543
_shelx_shelxl_version_number     2018/3
_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   0.857
_shelx_estimated_absorpt_t_max   0.914
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 0.47360(2) 0.94721(2) 0.43213(5) 0.0580(3) Uani 1 2 d S T P . .
O1 O 0.51706(15) 0.91601(13) 0.5435(3) 0.0791(8) Uani 1 1 d . . . . .
O2 O 0.56077(16) 1.00495(13) 0.6607(3) 0.0814(8) Uani 1 1 d . . . . .
O3 O 0.43224(12) 0.8645(2) 0.3064(6) 0.1075(17) Uani 1 2 d S T P . .
H3O H 0.411517 0.823034 0.341814 0.129 Uiso 1 2 calc R U P . .
N1 N 0.6529(4) 0.8264(2) 0.9233(7) 0.150(4) Uani 1 2 d S T P . .
H1 H 0.677765 0.838883 0.986182 0.180 Uiso 1 2 calc R U P . .
C1 C 0.55025(19) 0.94857(16) 0.6335(3) 0.0718(9) Uani 1 1 d . . . . .
C2 C 0.5777(2) 0.91776(17) 0.7126(4) 0.0804(10) Uani 1 1 d . . . . .
C3 C 0.6156(3) 0.9516(2) 0.8147(6) 0.1133(19) Uani 1 1 d . . . . .
H3 H 0.622292 0.993248 0.831897 0.136 Uiso 1 1 calc R U . . .
C4 C 0.6420(4) 0.9257(3) 0.8873(6) 0.135(3) Uani 1 1 d . . . . .
H4 H 0.668230 0.949745 0.952204 0.162 Uiso 1 1 calc R U . . .
C5 C 0.6298(3) 0.8626(3) 0.8649(5) 0.1099(19) Uani 1 1 d . . . . .
C6 C 0.5948(3) 0.82836(19) 0.7609(5) 0.0911(14) Uani 1 1 d . . . . .
C7 C 0.5680(2) 0.85573(17) 0.6869(4) 0.0769(11) Uani 1 1 d . . . . .
H7 H 0.543478 0.832778 0.619673 0.092 Uiso 1 1 calc R U . . .
C8 C 0.4326(4) 0.8652(8) 0.2085(15) 0.271(11) Uani 1 2 d S T P . .
H8A H 0.479533 0.894314 0.199453 0.325 Uiso 0.5 1 calc R U P . .
H8B H 0.414781 0.894314 0.199453 0.325 Uiso 0.5 1 calc R U P . .
C9 C 0.4229(4) 0.8457(8) 0.1091(13) 0.293(12) Uani 1 2 d S T P . .
H9A H 0.441094 0.882189 0.054073 0.440 Uiso 1 2 calc R U P . .
H9B H 0.443078 0.819489 0.095816 0.440 Uiso 0.5 1 calc R U P . .
H9C H 0.376411 0.819489 0.095816 0.440 Uiso 0.5 1 calc R U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0060 0.0030 '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 0.0100 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0180 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.1640 1.8640 '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
_geom_angle_publ_flag
O1 Cu1 O1 90.15(19) . 11 ?
O1 Cu1 O2 89.67(14) . 5_676 ?
O1 Cu1 O2 168.42(12) 11 5_676 ?
O1 Cu1 O2 168.42(12) . 7_676 ?
O1 Cu1 O2 89.66(14) 11 7_676 ?
O2 Cu1 O2 88.2(2) 5_676 7_676 ?
O1 Cu1 O3 98.58(16) . . ?
O1 Cu1 O3 98.58(16) 11 . ?
O2 Cu1 O3 92.89(15) 5_676 . ?
O2 Cu1 O3 92.89(15) 7_676 . ?
O1 Cu1 Cu1 84.64(8) . 7_676 ?
O1 Cu1 Cu1 84.64(8) 11 7_676 ?
O2 Cu1 Cu1 83.82(8) 5_676 7_676 ?
O2 Cu1 Cu1 83.82(8) 7_676 7_676 ?
O3 Cu1 Cu1 175.40(17) . 7_676 ?
C1 O1 Cu1 123.3(2) . . ?
C1 O2 Cu1 123.9(3) . 7_676 ?
C8 O3 Cu1 128.7(9) . . ?
C5 N1 C5 109.1(5) . 12_565 ?
O2 C1 O1 124.4(4) . . ?
O2 C1 C2 118.2(3) . . ?
O1 C1 C2 117.4(3) . . ?
C7 C2 C3 118.8(4) . . ?
C7 C2 C1 120.9(3) . . ?
C3 C2 C1 120.3(4) . . ?
C4 C3 C2 122.0(4) . . ?
C3 C4 C5 119.1(4) . . ?
N1 C5 C4 130.1(5) . . ?
N1 C5 C6 109.2(4) . . ?
C4 C5 C6 120.4(4) . . ?
C7 C6 C5 119.5(4) . . ?
C7 C6 C6 134.3(2) . 12_565 ?
C5 C6 C6 106.2(3) . 12_565 ?
C6 C7 C2 119.9(4) . . ?
O3 C8 C9 159(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.961(3) . ?
Cu1 O1 1.961(3) 11 ?
Cu1 O2 1.970(3) 5_676 ?
Cu1 O2 1.970(3) 7_676 ?
Cu1 O3 2.184(5) . ?
Cu1 Cu1 2.6219(10) 7_676 ?
O1 C1 1.260(5) . ?
O2 C1 1.257(4) . ?
O3 C8 1.083(16) . ?
N1 C5 1.376(6) . ?
N1 C5 1.376(6) 12_565 ?
C1 C2 1.475(5) . ?
C2 C7 1.389(5) . ?
C2 C3 1.411(6) . ?
C3 C4 1.333(8) . ?
C4 C5 1.387(7) . ?
C5 C6 1.409(6) . ?
C6 C7 1.372(6) . ?
C6 C6 1.457(8) 12_565 ?
C8 C9 1.167(17) . ?
