#------------------------------------------------------------------------------
#$Date: 2016-11-08 21:33:45 +0200 (Tue, 08 Nov 2016) $
#$Revision: 188099 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/62/7226233.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_7226233
loop_
_publ_author_name
'Müller, Philipp'
'Grünker, Ronny'
'Bon, Volodymyr'
'Pfeffermann, Martin'
'Senkovska, Irena'
'Weiss, Manfred S.'
'Feng, Xinliang'
'Kaskel, Stefan'
_publ_section_title
;
 Topological control of 3,4-connected frameworks based on the
 Cu2-paddle-wheel node: tbo or pto, and why?
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              8164
_journal_paper_doi               10.1039/C6CE01513A
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C52 H32 Cu2 N1.33 O10'
_chemical_formula_weight         962.53
_chemical_name_systematic        DUT-64
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      cubic
_space_group_IT_number           223
_space_group_name_Hall           '-P 4n 2 3'
_space_group_name_H-M_alt        'P m -3 n'
_symmetry_space_group_name_Hall  '-P 4n 2 3'
_symmetry_space_group_name_H-M   'P m -3 n'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-05-19 deposited with the CCDC.
2016-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   35.490(4)
_cell_length_b                   35.490(4)
_cell_length_c                   35.490(4)
_cell_measurement_reflns_used    472
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      18.23
_cell_measurement_theta_min      2.48
_cell_volume                     44701(9)
_computing_cell_refinement       'mosflm 1.0.5'
_computing_data_collection       'marCCD 1994-2002'
_computing_data_reduction        scala
_computing_molecular_graphics    'Diamond 3.1'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'MX-225 CCD'
_diffrn_measurement_method       'Δφ scans'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.88561
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       1
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5818
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        23.532
_diffrn_reflns_theta_max         23.532
_diffrn_reflns_theta_min         1.430
_diffrn_source                   synchrotron
_diffrn_source_type              'BESSY BL MX-14.2'
_exptl_absorpt_coefficient_mu    0.275
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.215
_exptl_crystal_description       cuboctahedral
_exptl_crystal_F_000             2948
_exptl_crystal_recrystallization_method 'solvothermal synthesis'
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.110
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.021
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.827
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         3055
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      0.843
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.0771
_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)+(0.1879P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2502
_refine_ls_wR_factor_ref         0.2861
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1091
_reflns_number_total             3055
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ce01513a2.cif
_cod_data_source_block           pm3n_sqd
_cod_depositor_comments
'Adding full bibliography for 7226232--7226236.cif.'
_cod_original_cell_volume        44701(15)
_cod_database_code               7226233
_shelx_shelxl_version_number     2014/7
_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   0.978
_shelx_estimated_absorpt_t_max   0.978
_platon_squeeze_void_probe_radius 1.20
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, z+1/2, -y+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'x+1/2, -z+1/2, y+1/2'
'z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y-1/2, -x-1/2, z-1/2'
'y-1/2, x-1/2, z-1/2'
'-y-1/2, x-1/2, -z-1/2'
'y-1/2, -x-1/2, -z-1/2'
'-x-1/2, -z-1/2, y-1/2'
'x-1/2, -z-1/2, -y-1/2'
'x-1/2, z-1/2, y-1/2'
'-x-1/2, z-1/2, -y-1/2'
'-z-1/2, -y-1/2, x-1/2'
'-z-1/2, y-1/2, -x-1/2'
'z-1/2, -y-1/2, -x-1/2'
'z-1/2, y-1/2, x-1/2'
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
Cu1 Cu 0.5000 0.0000 0.21279(4) 0.283(2) Uani 1 4 d S T P
N1 N 0.2500 0.2500 0.2500 0.408(8) Uani 1 6 d DS T P
O2 O 0.5000 0.0000 0.14745(18) 0.364(4) Uani 1 4 d S T P
O1 O 0.46254(17) 0.03746(18) 0.21922(16) 0.317(3) Uani 1 1 d D . .
C1 C 0.4492(2) 0.0508(2) 0.2500 0.319(10) Uani 1 2 d DS T P
C2 C 0.4210(3) 0.0790(3) 0.2500 0.288(5) Uani 1 2 d DS T P
C3 C 0.4067(3) 0.0951(3) 0.2181(2) 0.351(4) Uani 1 1 d D . .
H3A H 0.4157 0.0872 0.1948 0.421 Uiso 1 1 calc R U .
C4 C 0.3770(3) 0.1251(3) 0.2191(3) 0.364(4) Uani 1 1 d D . .
H4A H 0.3694 0.1345 0.1959 0.437 Uiso 1 1 calc R U .
C5 C 0.3596(4) 0.1404(4) 0.2500 0.350(8) Uani 1 2 d DS T P
C6 C 0.3313(3) 0.1687(3) 0.2500 0.341(8) Uani 1 2 d DS T P
C7 C 0.3198(3) 0.1785(3) 0.2141(3) 0.424(6) Uani 1 1 d D . .
H7A H 0.3293 0.1685 0.1919 0.508 Uiso 1 1 calc R U .
C8 C 0.2932(3) 0.2044(3) 0.2164(2) 0.424(6) Uani 1 1 d D . .
H8A H 0.2826 0.2128 0.1940 0.509 Uiso 1 1 calc R U .
C9 C 0.27945(17) 0.22055(17) 0.2500 0.420(9) Uani 1 2 d DS 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 0.0060 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'
Cu Cu 0.1640 1.8640 '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'
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
O1 Cu1 O1 166.1(4) 28_655 27
O1 Cu1 O1 89.2(4) 28_655 2_655
O1 Cu1 O1 89.2(4) 27 2_655
O1 Cu1 O1 89.2(4) 28_655 .
O1 Cu1 O1 89.2(4) 27 .
O1 Cu1 O1 166.2(4) 2_655 .
O1 Cu1 O2 96.93(18) 28_655 .
O1 Cu1 O2 96.93(18) 27 .
O1 Cu1 O2 96.93(18) 2_655 .
O1 Cu1 O2 96.92(18) . .
O1 Cu1 Cu1 83.07(18) 28_655 13_545
O1 Cu1 Cu1 83.07(18) 27 13_545
O1 Cu1 Cu1 83.07(18) 2_655 13_545
O1 Cu1 Cu1 83.08(18) . 13_545
O2 Cu1 Cu1 180.0 . 13_545
C9 N1 C9 120.0 9 5
C9 N1 C9 120.0 9 .
C9 N1 C9 120.000(2) 5 .
C1 O1 Cu1 128.5(7) . .
O1 C1 O1 116.9(11) 14 .
O1 C1 C2 121.6(5) 14 .
O1 C1 C2 121.6(5) . .
C3 C2 C3 112.0(12) 14 .
C3 C2 C1 124.0(6) 14 .
C3 C2 C1 124.0(6) . .
C2 C3 C4 122.6(10) . .
C2 C3 H3A 118.7 . .
C4 C3 H3A 118.7 . .
C5 C4 C3 128.2(12) . .
C5 C4 H4A 115.9 . .
C3 C4 H4A 115.9 . .
C4 C5 C4 106.4(16) 14 .
C4 C5 C6 126.8(8) 14 .
C4 C5 C6 126.8(8) . .
C7 C6 C7 134.4(15) 14 .
C7 C6 C5 112.8(8) 14 .
C7 C6 C5 112.8(8) . .
C8 C7 C6 109.3(13) . .
C8 C7 H7A 125.4 . .
C6 C7 H7A 125.4 . .
C7 C8 C9 125.6(10) . .
C7 C8 H8A 117.2 . .
C9 C8 H8A 117.2 . .
C8 C9 C8 115.8(10) 14 .
C8 C9 N1 122.1(5) 14 .
C8 C9 N1 122.1(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.894(6) 28_655
Cu1 O1 1.894(6) 27
Cu1 O1 1.894(6) 2_655
Cu1 O1 1.894(6) .
Cu1 O2 2.319(6) .
Cu1 Cu1 2.642(3) 13_545
N1 C9 1.478(8) 9
N1 C9 1.478(8) 5
N1 C9 1.478(8) .
O1 C1 1.282(5) .
C1 O1 1.282(5) 14
C1 C2 1.415(12) .
C2 C3 1.366(6) 14
C2 C3 1.366(6) .
C3 C4 1.496(9) .
C3 H3A 0.9300 .
C4 C5 1.370(8) .
C4 H4A 0.9300 .
C5 C4 1.370(8) 14
C5 C6 1.421(14) .
C6 C7 1.382(7) 14
C6 C7 1.382(7) .
C7 C8 1.320(8) .
C7 H7A 0.9300 .
C8 C9 1.408(6) .
C8 H8A 0.9300 .
C9 C8 1.408(6) 14
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 -0.003 -0.008 -0.004 39955 6923 '27 DMF molecules per formula unit '
