data_NbU-1
_audit_creation_date               2018-08-23
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2014/7'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst., 40, 786-790;
Palatinus, L. & van der Lee, A. (2008). J. Appl. Cryst. 41, 975-984;
Palatinus, L., Prathapa, S. J. & van Smaalen, S. (2012). J. Appl. Cryst. 45,
 575-580.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           '0.13(C480 H480 Cu136 N480 O96)'
_chemical_formula_sum              'C60 H60 Cu17 N60 O12'
_chemical_formula_weight           2893.86
_chemical_melting_point            ?
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'
 'N' 'N' 0.0061 0.0033 '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'

_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.
;
_space_group_crystal_system        'cubic'
_space_group_IT_number             230
_space_group_name_H-M_alt          'I a -3 d'
_space_group_name_Hall             '-I 4bd 2c 3'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x, y+1/2, -z+1/2'
 'x+1/2, -y+1/2, -z'
 'z, x, y'
 'z+1/2, -x+1/2, -y'
 '-z+1/2, -x, y+1/2'
 '-z, x+1/2, -y+1/2'
 'y, z, x'
 '-y, z+1/2, -x+1/2'
 'y+1/2, -z+1/2, -x'
 '-y+1/2, -z, x+1/2'
 'y+3/4, x+1/4, -z+1/4'
 '-y+3/4, -x+3/4, -z+3/4'
 'y+1/4, -x+1/4, z+3/4'
 '-y+1/4, x+3/4, z+1/4'
 'x+3/4, z+1/4, -y+1/4'
 '-x+1/4, z+3/4, y+1/4'
 '-x+3/4, -z+3/4, -y+3/4'
 'x+1/4, -z+1/4, y+3/4'
 'z+3/4, y+1/4, -x+1/4'
 'z+1/4, -y+1/4, x+3/4'
 '-z+1/4, y+3/4, x+1/4'
 '-z+3/4, -y+3/4, -x+3/4'
 'x+1/2, y+1/2, z+1/2'
 '-x+1, -y+1/2, z+1'
 '-x+1/2, y+1, -z+1'
 'x+1, -y+1, -z+1/2'
 'z+1/2, x+1/2, y+1/2'
 'z+1, -x+1, -y+1/2'
 '-z+1, -x+1/2, y+1'
 '-z+1/2, x+1, -y+1'
 'y+1/2, z+1/2, x+1/2'
 '-y+1/2, z+1, -x+1'
 'y+1, -z+1, -x+1/2'
 '-y+1, -z+1/2, x+1'
 'y+5/4, x+3/4, -z+3/4'
 '-y+5/4, -x+5/4, -z+5/4'
 'y+3/4, -x+3/4, z+5/4'
 '-y+3/4, x+5/4, z+3/4'
 'x+5/4, z+3/4, -y+3/4'
 '-x+3/4, z+5/4, y+3/4'
 '-x+5/4, -z+5/4, -y+5/4'
 'x+3/4, -z+3/4, y+5/4'
 'z+5/4, y+3/4, -x+3/4'
 'z+3/4, -y+3/4, x+5/4'
 '-z+3/4, y+5/4, x+3/4'
 '-z+5/4, -y+5/4, -x+5/4'
 '-x, -y, -z'
 'x-1/2, y, -z-1/2'
 'x, -y-1/2, z-1/2'
 '-x-1/2, y-1/2, z'
 '-z, -x, -y'
 '-z-1/2, x-1/2, y'
 'z-1/2, x, -y-1/2'
 'z, -x-1/2, y-1/2'
 '-y, -z, -x'
 'y, -z-1/2, x-1/2'
 '-y-1/2, z-1/2, x'
 'y-1/2, z, -x-1/2'
 '-y-3/4, -x-1/4, z-1/4'
 'y-3/4, x-3/4, z-3/4'
 '-y-1/4, x-1/4, -z-3/4'
 'y-1/4, -x-3/4, -z-1/4'
 '-x-3/4, -z-1/4, y-1/4'
 'x-1/4, -z-3/4, -y-1/4'
 'x-3/4, z-3/4, y-3/4'
 '-x-1/4, z-1/4, -y-3/4'
 '-z-3/4, -y-1/4, x-1/4'
 '-z-1/4, y-1/4, -x-3/4'
 'z-1/4, -y-3/4, -x-1/4'
 'z-3/4, y-3/4, x-3/4'
 '-x+1/2, -y+1/2, -z+1/2'
 'x, y+1/2, -z'
 'x+1/2, -y, z'
 '-x, y, z+1/2'
 '-z+1/2, -x+1/2, -y+1/2'
 '-z, x, y+1/2'
 'z, x+1/2, -y'
 'z+1/2, -x, y'
 '-y+1/2, -z+1/2, -x+1/2'
 'y+1/2, -z, x'
 '-y, z, x+1/2'
 'y, z+1/2, -x'
 '-y-1/4, -x+1/4, z+1/4'
 'y-1/4, x-1/4, z-1/4'
 '-y+1/4, x+1/4, -z-1/4'
 'y+1/4, -x-1/4, -z+1/4'
 '-x-1/4, -z+1/4, y+1/4'
 'x+1/4, -z-1/4, -y+1/4'
 'x-1/4, z-1/4, y-1/4'
 '-x+1/4, z+1/4, -y-1/4'
 '-z-1/4, -y+1/4, x+1/4'
 '-z+1/4, y+1/4, -x-1/4'
 'z+1/4, -y-1/4, -x+1/4'
 'z-1/4, y-1/4, x-1/4'

_cell_length_a                     31.272(4)
_cell_length_b                     31.272(4)
_cell_length_c                     31.272(4)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  90
_cell_volume                       30581(11)
_cell_formula_units_Z              8
_cell_measurement_reflns_used      588140
_cell_measurement_temperature      293(2)
_cell_measurement_theta_max        28.0870
_cell_measurement_theta_min        3.6530
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      2.364
_exptl_absorpt_correction_T_max    ?
_exptl_absorpt_correction_T_min    ?
_exptl_absorpt_correction_type     'none'
_exptl_absorpt_process_details     ?
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              green
_exptl_crystal_density_diffrn      1.257
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               11432
_exptl_crystal_size_max            0.2
_exptl_crystal_size_mid            0.2
_exptl_crystal_size_min            0.1
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0380
_diffrn_reflns_av_unetI/netI       0.0105
_diffrn_reflns_Laue_measured_fraction_full  0.997
_diffrn_reflns_Laue_measured_fraction_max  0.998
_diffrn_reflns_limit_h_max         42
_diffrn_reflns_limit_h_min         -35
_diffrn_reflns_limit_k_max         42
_diffrn_reflns_limit_k_min         -34
_diffrn_reflns_limit_l_max         34
_diffrn_reflns_limit_l_min         -42
_diffrn_reflns_number              72448
_diffrn_reflns_point_group_measured_fraction_full  0.997
_diffrn_reflns_point_group_measured_fraction_max  0.998
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           29.173
_diffrn_reflns_theta_min           2.437
_diffrn_ambient_temperature        293(2)
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.997
_diffrn_measured_fraction_theta_max  0.998
_diffrn_measurement_device_type    'Bruker APEX-II CCD'
_diffrn_measurement_method         'ω scans'
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     ?
_diffrn_standards_number           0
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  2985
_reflns_number_total               3452
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         ?
_computing_data_collection         ?
_computing_data_reduction          ?
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max           0.845
_refine_diff_density_min           -0.449
_refine_diff_density_rms           0.067
_refine_ls_extinction_coef         0.00014(4)
_refine_ls_extinction_expression  
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_extinction_method       'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref     1.183
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       115
_refine_ls_number_reflns           3452
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0735
_refine_ls_R_factor_gt             0.0622
_refine_ls_restrained_S_all        1.183
_refine_ls_shift/su_max            0.002
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0887P)²+34.2722P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1830
_refine_ls_wR_factor_ref           0.1953
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups, All O(H) groups
2.a Rotating group:
 N3(H3A,H3B)
2.b Ternary CH refined with riding coordinates:
 O1(H1)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       iterative
_atom_sites_solution_secondary     ?
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
 Cu3 Cu 0.5000 0.7500 0.3750 0.0702(3) Uani 1 4 d S T P . .
 Cu1 Cu 0.5000 1.0000 0.5000 0.0726(4) Uani 1 6 d S T P . .
 Cu2 Cu 0.56761(2) 0.92781(2) 0.50271(2) 0.0848(3) Uani 1 1 d . . . . .
 O1 O 0.50726(10) 0.93475(12) 0.49043(11) 0.0908(10) Uani 1 1 d . . . . .
 H1 H 0.4877 0.9162 0.5064 0.109 Uiso 1 1 calc R . . . .
 N2 N 0.51410(9) 0.80120(10) 0.41116(10) 0.0688(7) Uani 1 1 d . . . . .
 N1 N 0.51737(11) 0.87202(11) 0.42795(10) 0.0751(8) Uani 1 1 d . . . . .
 N5 N 0.56357(10) 0.86562(12) 0.49024(11) 0.0787(9) Uani 1 1 d . . . . .
 N4 N 0.58230(12) 0.79351(13) 0.50800(12) 0.0840(9) Uani 1 1 d . . . . .
 N3 N 0.56157(12) 0.73575(12) 0.46650(14) 0.0926(11) Uani 1 1 d . . . . .
 H3A H 0.5619 0.7223 0.4908 0.111 Uiso 1 1 d GR . . . .
 H3B H 0.5389 0.7283 0.4524 0.111 Uiso 1 1 d GR . . . .
 C1 C 0.54136(11) 0.84966(13) 0.45710(12) 0.0698(8) Uani 1 1 d . . . . .
 C2 C 0.50173(12) 0.84085(12) 0.40203(12) 0.0711(9) Uani 1 1 d . . . . .
 H2 H 0.4835 0.8469 0.3793 0.085 Uiso 1 1 calc R . . . .
 C3 C 0.53958(11) 0.80680(13) 0.44714(12) 0.0687(8) Uani 1 1 d . . . . .
 C4 C 0.56066(12) 0.77747(14) 0.47308(13) 0.0748(9) Uani 1 1 d . . . . .
 C5 C 0.58266(14) 0.83472(16) 0.51412(14) 0.0829(11) Uani 1 1 d . . . . .
 H5 H 0.5979 0.8442 0.5378 0.099 Uiso 1 1 calc R . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
 Cu3 N2 2.009(3) . ?
 Cu3 N2 2.009(3) 64_576 ?
 Cu3 N2 2.009(3) 87_656 ?
 Cu3 N2 2.009(3) 26_564 ?
 Cu1 O1 2.075(3) . ?
 Cu1 O1 2.075(3) 49_676 ?
 Cu1 O1 2.075(3) 11_466 ?
 Cu1 O1 2.075(3) 8_656 ?
 Cu1 O1 2.075(3) 56_575 ?
 Cu1 O1 2.075(3) 59_765 ?
 Cu2 O1 1.938(3) . ?
 Cu2 O1 1.965(3) 59_765 ?
 Cu2 N1 1.943(3) 59_765 ?
 Cu2 N5 1.988(4) . ?
 O1 Cu2 1.965(3) 56_575 ?
 O1 H1 0.9800 . ?
 N2 C2 1.330(5) . ?
 N2 C3 1.390(5) . ?
 N1 Cu2 1.943(3) 56_575 ?
 N1 C1 1.372(5) . ?
 N1 C2 1.359(5) . ?
 N5 C1 1.344(5) . ?
 N5 C5 1.359(6) . ?
 N4 C4 1.379(5) . ?
 N4 C5 1.303(6) . ?
 N3 H3A 0.8684 . ?
 N3 H3B 0.8660 . ?
 N3 C4 1.321(6) . ?
 C1 C3 1.377(6) . ?
 C2 H2 0.9300 . ?
 C3 C4 1.391(6) . ?
 C5 H5 0.9300 . ?

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
 N2 Cu3 N2 108.47(9) . 87_656 ?
 N2 Cu3 N2 108.47(9) 87_656 26_564 ?
 N2 Cu3 N2 111.50(19) . 26_564 ?
 N2 Cu3 N2 108.46(9) . 64_576 ?
 N2 Cu3 N2 111.50(19) 87_656 64_576 ?
 N2 Cu3 N2 108.47(9) 64_576 26_564 ?
 O1 Cu1 O1 76.48(14) 56_575 11_466 ?
 O1 Cu1 O1 76.48(14) 8_656 59_765 ?
 O1 Cu1 O1 76.48(14) 59_765 . ?
 O1 Cu1 O1 76.48(14) 49_676 11_466 ?
 O1 Cu1 O1 103.52(14) 49_676 59_765 ?
 O1 Cu1 O1 103.52(14) 8_656 . ?
 O1 Cu1 O1 103.52(14) 8_656 11_466 ?
 O1 Cu1 O1 180.0 56_575 8_656 ?
 O1 Cu1 O1 76.48(14) 56_575 . ?
 O1 Cu1 O1 103.52(14) 56_575 49_676 ?
 O1 Cu1 O1 180.0 49_676 . ?
 O1 Cu1 O1 76.48(14) 8_656 49_676 ?
 O1 Cu1 O1 103.52(14) 11_466 . ?
 O1 Cu1 O1 103.52(14) 56_575 59_765 ?
 O1 Cu1 O1 180.0 59_765 11_466 ?
 O1 Cu2 O1 82.3(2) . 59_765 ?
 O1 Cu2 N1 173.11(14) . 59_765 ?
 O1 Cu2 N5 90.50(14) . . ?
 O1 Cu2 N5 170.77(13) 59_765 . ?
 N1 Cu2 O1 90.99(13) 59_765 59_765 ?
 N1 Cu2 N5 96.33(13) 59_765 . ?
 Cu1 O1 H1 116.1 . . ?
 Cu2 O1 Cu1 99.96(18) 56_575 . ?
 Cu2 O1 Cu1 100.84(16) . . ?
 Cu2 O1 Cu2 105.30(17) . 56_575 ?
 Cu2 O1 H1 116.1 56_575 . ?
 Cu2 O1 H1 116.1 . . ?
 C2 N2 Cu3 124.0(2) . . ?
 C2 N2 C3 102.9(3) . . ?
 C3 N2 Cu3 133.0(3) . . ?
 C1 N1 Cu2 128.7(3) . 56_575 ?
 C2 N1 Cu2 127.7(3) . 56_575 ?
 C2 N1 C1 103.1(3) . . ?
 C1 N5 Cu2 123.2(3) . . ?
 C1 N5 C5 112.7(4) . . ?
 C5 N5 Cu2 124.0(3) . . ?
 C5 N4 C4 118.7(4) . . ?
 H3A N3 H3B 109.0 . . ?
 C4 N3 H3A 110.1 . . ?
 C4 N3 H3B 109.1 . . ?
 N1 C1 C3 108.9(3) . . ?
 N5 C1 N1 127.3(4) . . ?
 N5 C1 C3 123.8(4) . . ?
 N2 C2 N1 115.9(3) . . ?
 N2 C2 H2 122.1 . . ?
 N1 C2 H2 122.1 . . ?
 N2 C3 C4 131.4(4) . . ?
 C1 C3 N2 109.2(3) . . ?
 C1 C3 C4 119.4(4) . . ?
 N4 C4 C3 117.0(4) . . ?
 N3 C4 N4 118.1(4) . . ?
 N3 C4 C3 124.8(4) . . ?
 N5 C5 H5 115.9 . . ?
 N4 C5 N5 128.2(4) . . ?
 N4 C5 H5 115.9 . . ?

_olex2_submission_special_instructions  'No special instructions were received'

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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  0.164  0.047  0.116      8025      1623 ' '
   2  0.672 -0.053  0.095      8025      1623 ' '
_platon_squeeze_details                           ?

