#------------------------------------------------------------------------------
#$Date: 2016-11-08 21:33:45 +0200 (Tue, 08 Nov 2016) $
#$Revision: 188099 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/62/7226235.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_7226235
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            'C68 H48 Cu3 N5.33 O10'
_chemical_formula_weight         1290.40
_chemical_name_systematic        DUT-125
_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                   35.510(4)
_cell_length_b                   35.510(4)
_cell_length_c                   35.510(4)
_cell_measurement_reflns_used    685
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      3.98
_cell_volume                     44777(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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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     0.89500
_diffrn_reflns_av_R_equivalents  0.1076
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            94817
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        28.101
_diffrn_reflns_theta_max         28.101
_diffrn_reflns_theta_min         1.021
_diffrn_source                   synchrotron
_diffrn_source_type              'BESSY BL MX-14.2'
_exptl_absorpt_coefficient_mu    0.418
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.287
_exptl_crystal_description       cubic
_exptl_crystal_F_000             3962
_exptl_crystal_recrystallization_method 'post-synthetic functionalization'
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         4827
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0673
_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)+(0.1584P)²+4.8475P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1999
_refine_ls_wR_factor_ref         0.2455
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3267
_reflns_number_total             4827
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ce01513a2.cif
_cod_data_source_block           pm3n_a_sq
_cod_depositor_comments
'Adding full bibliography for 7226232--7226236.cif.'
_cod_original_cell_volume        44777(16)
_cod_database_code               7226235
_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   0.979
_shelx_estimated_absorpt_t_max   0.979
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 0.0000 0.5000 0.71224(2) 0.0701(4) Uani 1 4 d S T P
O1 O 0.03881(6) 0.53873(6) 0.71846(6) 0.0965(8) Uani 1 1 d . . .
C1 C 0.05043(10) 0.55043(10) 0.7500 0.0875(13) Uani 1 2 d S T P
C2 C 0.08019(9) 0.58019(9) 0.7500 0.0992(14) Uani 1 2 d S T P
C3 C 0.09576(14) 0.59303(13) 0.78274(11) 0.158(2) Uani 1 1 d . . .
H3A H 0.0880 0.5828 0.8056 0.190 Uiso 1 1 calc R U .
C4 C 0.12315(15) 0.62115(15) 0.78250(12) 0.180(3) Uani 1 1 d . . .
H4A H 0.1327 0.6297 0.8053 0.216 Uiso 1 1 calc R U .
C5 C 0.13643(12) 0.63643(12) 0.7500 0.136(2) Uani 1 2 d S T P
C6 C 0.16615(12) 0.66615(12) 0.7500 0.158(3) Uani 1 2 d S T P
C7 C 0.17812(17) 0.68228(17) 0.78259(14) 0.200(3) Uani 1 1 d . . .
H7A H 0.1678 0.6746 0.8054 0.239 Uiso 1 1 calc R U .
C8 C 0.20539(18) 0.71002(18) 0.78218(16) 0.215(4) Uani 1 1 d . . .
H8A H 0.2128 0.7211 0.8047 0.258 Uiso 1 1 calc R U .
C9 C 0.22125(13) 0.72125(13) 0.7500 0.188(4) Uani 1 2 d S T P
N1 N 0.2500 0.7500 0.7500 0.233(8) Uani 1 6 d S T P
Cu2 Cu 0.02462(12) 0.5000 0.5000 0.146(2) Uani 0.32 4 d DS T P
N2 N 0.0000 0.5000 0.65282(13) 0.1033(18) Uani 1 4 d DS TU P
C12 C 0.0000 0.5000 0.5744(2) 0.258(7) Uani 1 4 d DS TU P
O2 O 0.0000 0.5000 0.53822(13) 0.341(7) Uani 1 4 d DS TU P
C10 C 0.0303(2) 0.5000 0.63334(18) 0.195(5) Uani 0.64 2 d DS TU P
H10A H 0.0532 0.5000 0.6461 0.234 Uiso 0.64 2 calc R U P
C11 C 0.0311(2) 0.5000 0.5932(2) 0.277(7) Uani 0.64 2 d DS TU P
C13 C 0.0690(4) 0.5000 0.5754(3) 0.424(11) Uani 0.64 2 d DS TU P
H13A H 0.0919 0.5000 0.5881 0.508 Uiso 0.64 2 calc R U P
N3 N 0.0643(5) 0.5000 0.5363(3) 0.511(12) Uani 0.64 2 d DS TU P
C14 C 0.1029(5) 0.5000 0.5199(2) 0.561(16) Uani 0.64 2 d DS TU P
H14A H 0.1163 0.5221 0.5288 0.673 Uiso 0.32 1 calc R U P
H14B H 0.1163 0.4779 0.5288 0.673 Uiso 0.32 1 calc R U P
Cu3 Cu 0.0000 0.5265(3) 0.5000 0.167(5) Uani 0.18 4 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 0.1490 1.8970 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0110 0.0060 '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 89.15(13) 2_565 28
O1 Cu1 O1 89.39(13) 2_565 27_565
O1 Cu1 O1 167.06(12) 28 27_565
O1 Cu1 O1 167.06(12) 2_565 .
O1 Cu1 O1 89.39(14) 28 .
O1 Cu1 O1 89.15(13) 27_565 .
O1 Cu1 N2 96.47(6) 2_565 .
O1 Cu1 N2 96.47(6) 28 .
O1 Cu1 N2 96.47(6) 27_565 .
O1 Cu1 N2 96.47(6) . .
O1 Cu1 Cu1 83.53(6) 2_565 13_456
O1 Cu1 Cu1 83.53(6) 28 13_456
O1 Cu1 Cu1 83.53(6) 27_565 13_456
O1 Cu1 Cu1 83.53(6) . 13_456
N2 Cu1 Cu1 180.0 . 13_456
C1 O1 Cu1 124.1(2) . .
O1 C1 O1 124.8(4) . 13_456
O1 C1 C2 117.6(2) . .
O1 C1 C2 117.6(2) 13_456 .
C3 C2 C3 117.0(5) . 13_456
C3 C2 C1 121.5(3) . .
C3 C2 C1 121.5(3) 13_456 .
C2 C3 C4 121.1(4) . .
C2 C3 H3A 119.5 . .
C4 C3 H3A 119.5 . .
C5 C4 C3 122.2(4) . .
C5 C4 H4A 118.9 . .
C3 C4 H4A 118.9 . .
C4 C5 C4 116.3(6) . 13_456
C4 C5 C6 121.8(3) . .
C4 C5 C6 121.8(3) 13_456 .
C7 C6 C7 117.5(6) . 13_456
C7 C6 C5 121.3(3) . .
C7 C6 C5 121.3(3) 13_456 .
C6 C7 C8 120.7(5) . .
C6 C7 H7A 119.6 . .
C8 C7 H7A 119.6 . .
C9 C8 C7 121.2(6) . .
C9 C8 H8A 119.4 . .
C7 C8 H8A 119.4 . .
C8 C9 C8 118.7(7) . 13_456
C8 C9 N1 120.6(3) . .
C8 C9 N1 120.6(3) 13_456 .
C9 N1 C9 120.000(1) 10_656 7_665
C9 N1 C9 120.000(1) 10_656 .
C9 N1 C9 120.000(1) 7_665 .
Cu3 Cu2 Cu3 94.3(8) 25_566 .
Cu3 Cu2 O2 68.4(2) 25_566 25_566
Cu3 Cu2 O2 68.4(2) . 25_566
Cu3 Cu2 O2 68.4(2) 25_566 .
Cu3 Cu2 O2 68.4(2) . .
O2 Cu2 O2 114.4(3) 25_566 .
Cu3 Cu2 Cu2 47.1(4) 25_566 25_566
Cu3 Cu2 Cu2 47.1(4) . 25_566
O2 Cu2 Cu2 57.22(16) 25_566 25_566
O2 Cu2 Cu2 57.22(16) . 25_566
Cu3 Cu2 N3 120.1(3) 25_566 .
Cu3 Cu2 N3 120.1(3) . .
O2 Cu2 N3 165.3(4) 25_566 .
O2 Cu2 N3 80.3(4) . .
Cu2 Cu2 N3 137.5(4) 25_566 .
Cu3 Cu2 N3 120.1(3) 25_566 26_556
Cu3 Cu2 N3 120.1(3) . 26_556
O2 Cu2 N3 80.3(4) 25_566 26_556
O2 Cu2 N3 165.3(4) . 26_556
Cu2 Cu2 N3 137.5(4) 25_566 26_556
N3 Cu2 N3 85.0(8) . 26_556
C10 N2 C10 114.5(7) 2_565 .
C10 N2 Cu1 122.8(4) 2_565 .
C10 N2 Cu1 122.8(4) . .
O2 C12 C11 121.2(4) . .
O2 C12 C11 121.2(4) . 2_565
C11 C12 C11 117.6(9) . 2_565
C12 O2 Cu2 147.22(16) . 25_566
C12 O2 Cu2 147.22(16) . .
Cu2 O2 Cu2 65.6(3) 25_566 .
C12 O2 Cu3 145.2(3) . 25_566
Cu2 O2 Cu3 46.32(19) 25_566 25_566
Cu2 O2 Cu3 46.32(19) . 25_566
C12 O2 Cu3 145.2(3) . .
Cu2 O2 Cu3 46.32(19) 25_566 .
Cu2 O2 Cu3 46.32(19) . .
Cu3 O2 Cu3 69.5(6) 25_566 .
N2 C10 C11 123.9(6) . .
N2 C10 H10A 118.1 . .
C11 C10 H10A 118.1 . .
C12 C11 C10 120.1(6) . .
C12 C11 C13 123.6(8) . .
C10 C11 C13 116.3(7) . .
N3 C13 C11 108.3(13) . .
N3 C13 H13A 125.8 . .
C11 C13 H13A 125.8 . .
C13 N3 C14 106.2(12) . .
C13 N3 Cu2 139.4(12) . .
C14 N3 Cu2 114.5(8) . .
C14 C14 N3 113.0(6) 26_556 .
C14 C14 H14A 109.0 26_556 .
N3 C14 H14A 109.0 . .
C14 C14 H14B 109.0 26_556 .
N3 C14 H14B 109.0 . .
H14A C14 H14B 107.8 . .
Cu2 Cu3 Cu2 85.7(8) 25_566 .
Cu2 Cu3 O2 65.3(3) 25_566 25_566
Cu2 Cu3 O2 65.3(3) . 25_566
Cu2 Cu3 O2 65.3(3) 25_566 .
Cu2 Cu3 O2 65.3(3) . .
O2 Cu3 O2 110.5(6) 25_566 .
Cu2 Cu3 Cu3 42.9(4) 25_566 25_566
Cu2 Cu3 Cu3 42.9(4) . 25_566
O2 Cu3 Cu3 55.2(3) 25_566 25_566
O2 Cu3 Cu3 55.2(3) . 25_566
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.959(2) 2_565
Cu1 O1 1.959(2) 28
Cu1 O1 1.959(2) 27_565
Cu1 O1 1.959(2) .
Cu1 N2 2.110(5) .
Cu1 Cu1 2.6813(11) 13_456
O1 C1 1.264(3) .
C1 O1 1.264(3) 13_456
C1 C2 1.495(6) .
C2 C3 1.366(4) .
C2 C3 1.366(4) 13_456
C3 C4 1.394(6) .
C3 H3A 0.9300 .
C4 C5 1.360(5) .
C4 H4A 0.9300 .
C5 C4 1.360(5) 13_456
C5 C6 1.492(8) .
C6 C7 1.359(5) .
C6 C7 1.359(5) 13_456
C7 C8 1.381(6) .
C7 H7A 0.9300 .
C8 C9 1.335(6) .
C8 H8A 0.9300 .
C9 C8 1.335(6) 13_456
C9 N1 1.444(7) .
N1 C9 1.444(7) 10_656
N1 C9 1.444(7) 7_665
Cu2 Cu3 1.285(6) 25_566
Cu2 Cu3 1.285(6) .
Cu2 O2 1.614(5) 25_566
Cu2 O2 1.614(5) .
Cu2 Cu2 1.748(9) 25_566
Cu2 N3 1.910(15) .
Cu2 N3 1.910(15) 26_556
N2 C10 1.279(7) 2_565
N2 C10 1.279(7) .
C12 O2 1.284(9) .
C12 C11 1.289(9) .
C12 C11 1.289(9) 2_565
O2 Cu2 1.614(5) 25_566
O2 Cu3 1.652(6) 25_566
O2 Cu3 1.652(6) .
C10 C11 1.426(9) .
C10 H10A 0.9300 .
C11 C13 1.488(13) .
C13 N3 1.396(13) .
C13 H13A 0.9300 .
N3 C14 1.490(15) .
C14 C14 1.414(16) 26_556
C14 H14A 0.9700 .
C14 H14B 0.9700 .
Cu3 Cu2 1.285(6) 25_566
Cu3 O2 1.652(6) 25_566
Cu3 Cu3 1.885(19) 25_566
