#------------------------------------------------------------------------------
#$Date: 2019-11-25 02:46:47 +0200 (Mon, 25 Nov 2019) $
#$Revision: 239980 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/06/4350668.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_4350668
loop_
_publ_author_name
'Weng, Zhehui'
'Zhang, Zhi-hui'
'Olds, Travis'
'Sterniczuk, Marcin'
'Burns, Peter C.'
_publ_section_title
;
 Copper(I) and copper(II) uranyl heterometallic hybrid materials.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7993
_journal_page_last               7998
_journal_paper_doi               10.1021/ic5007814
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C30 Cu N5 O18 U3, 3(O)'
_chemical_formula_sum            'C30 Cu N5 O21 U3'
_chemical_formula_weight         1543.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-02-14
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.11 svn.r2872 for OlexSys, GUI svn.r4767)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 105.0120(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.7137(11)
_cell_length_b                   14.5743(16)
_cell_length_c                   14.5114(16)
_cell_measurement_temperature    196(2)
_cell_volume                     1984.3(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      196.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21629
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.40
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    12.821
_exptl_crystal_density_diffrn    2.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1376
_refine_diff_density_max         1.140
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4065
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0219P)²+7.1994P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0681
_reflns_number_gt                3293
_reflns_number_total             4065
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5007814_si_002.cif
_cod_data_source_block           p2c_a
_cod_database_code               4350668
_olex2_refinement_description
;
1. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
2. Others
 Fixed Sof: O1AA(0.5) O2AA(0.5) O0AA(0.5)
;
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 '-x, -y, -z'
4 'x, -y, z-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_calc_flag
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.9144(7) 0.8493(5) 0.5673(5) 0.0219(15) Uani 1 d 1 . U .
C2 C 0.9862(7) 0.5726(4) 0.6433(5) 0.0201(15) Uani 1 d 1 . U .
C3 C 0.7738(8) 1.0859(5) 0.4838(6) 0.0258(16) Uani 1 d 1 . U .
C4 C 0.7820(7) 0.5087(5) 0.5340(5) 0.0218(15) Uani 1 d 1 . U .
C5 C 0.8182(7) 1.0020(5) 0.5445(5) 0.0249(15) Uani 1 d 1 . U .
C6 C 0.7123(8) 0.4304(5) 0.4700(5) 0.0252(16) Uani 1 d 1 . U .
C7 C 0.8677(8) 0.9241(5) 0.5069(5) 0.0243(16) Uani 1 d 1 . U .
C8 C 0.9259(7) 0.5000(5) 0.5875(5) 0.0238(15) Uani 1 d 1 . U .
C9 C 0.7747(7) 0.6563(5) 0.6031(5) 0.0216(15) Uani 1 d 1 . U .
C10 C 0.8462(8) 0.9219(5) 0.6917(5) 0.0252(16) Uani 1 d 1 . U .
C11 C 0.8065(8) 1.0013(5) 0.6385(6) 0.0310(17) Uani 1 d 1 . U .
C12 C 0.5000 0.7743(7) 0.2500 0.033(3) Uani 1 d 2 S TU P
C13 C 0.5000 0.6712(7) 0.2500 0.035(3) Uani 1 d 2 S TU P
C14 C 0.7079(7) 0.5880(5) 0.5410(5) 0.0228(15) Uani 1 d 1 . U .
C15 C 0.4849(9) 0.8205(6) 0.1639(7) 0.041(2) Uani 1 d 1 . U .
C16 C 0.4840(9) 0.9167(6) 0.1672(7) 0.045(2) Uani 1 d 1 . U .
N1 N 0.9046(6) 0.8481(4) 0.6584(4) 0.0216(13) Uani 1 d 1 . U .
N2 N 0.9123(6) 0.6489(4) 0.6530(4) 0.0177(12) Uani 1 d 1 . U .
N3 N 0.5000 0.9633(7) 0.2500 0.050(3) Uani 1 d 2 S TU P
O1 O 0.5000 0.3245(4) 0.2500 0.0203(14) Uani 1 d 2 S TU P
O2 O 0.7845(5) 0.2474(3) 0.3115(3) 0.0254(11) Uani 1 d 1 . U .
O3 O 0.5068(5) 0.2294(3) 0.4308(4) 0.0298(12) Uani 1 d 1 . U .
O4 O 0.5000 0.1477(4) 0.2500 0.0276(16) Uani 1 d 2 S TU P
O5 O 0.7880(6) 1.1636(3) 0.5215(4) 0.0334(13) Uani 1 d 1 . U .
O6 O 0.7209(6) 1.0760(3) 0.3959(4) 0.0322(13) Uani 1 d 1 . U .
O7 O 0.7741(6) 0.3557(4) 0.4759(4) 0.0423(14) Uani 1 d 1 . U .
O8 O 0.5901(6) 0.4449(4) 0.4131(4) 0.0367(13) Uani 1 d 1 . U .
O9 O 0.4697(7) 0.6288(4) 0.1722(4) 0.0503(17) Uani 1 d 1 . U .
O10 O 0.3202(5) 0.4813(4) 0.2557(4) 0.0354(13) Uani 1 d 1 . U .
Cu1 Cu 1.0000 0.74715(7) 0.7500 0.0167(2) Uani 1 d 2 S TU P
U1 U 0.63924(3) 0.237828(16) 0.366657(17) 0.01537(8) Uani 1 d 1 . U .
U2 U 0.5000 0.47866(2) 0.2500 0.01904(10) Uani 1 d 2 S TU P
O1AA O 0.830(3) 1.3014(18) 0.6975(18) 0.153(9) Uiso 0.50 d 1 . U .
O2AA O 0.942(4) 0.814(3) 0.318(3) 0.245(16) Uiso 0.50 d 1 . U .
O0AA O 1.122(4) 0.300(3) 0.616(3) 0.243(16) Uiso 0.50 d 1 . U .
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'
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'
U U -9.6767 9.6646 '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
N1 C1 C7 122.0(6) . .
N2 C2 C8 122.7(6) . .
C5 C3 U1 170.2(5) . 1_565
O5 C3 C5 119.9(7) . .
O5 C3 O6 121.3(7) . .
O5 C3 U1 62.9(4) . 1_565
O6 C3 C5 118.8(6) . .
O6 C3 U1 59.1(4) . 1_565
C8 C4 C6 119.2(7) . .
C14 C4 C6 121.1(6) . .
C14 C4 C8 119.6(6) . .
C7 C5 C3 120.4(6) . .
C11 C5 C3 119.6(7) . .
C11 C5 C7 119.9(7) . .
O7 C6 C4 119.3(7) . .
O7 C6 O8 123.0(7) . .
O8 C6 C4 117.7(7) . .
C5 C7 C1 118.4(7) . .
C2 C8 C4 117.7(6) . .
N2 C9 C14 121.5(6) . .
N1 C10 C11 122.8(7) . .
C10 C11 C5 117.9(7) . .
C15 C12 C13 118.9(5) 2_655 .
C15 C12 C13 118.9(5) . .
C15 C12 C15 122.2(10) 2_655 .
O9 C13 C12 119.5(5) . .
O9 C13 C12 119.5(5) 2_655 .
O9 C13 O9 120.9(10) 2_655 .
C4 C14 C9 119.0(6) . .
C12 C15 C16 116.9(9) . .
N3 C16 C15 122.1(9) . .
C1 N1 C10 118.6(6) . .
C1 N1 Cu1 120.8(5) . .
C10 N1 Cu1 120.0(5) . .
C2 N2 Cu1 120.9(4) . .
C9 N2 C2 119.3(6) . .
C9 N2 Cu1 119.6(5) . .
C16 N3 C16 119.7(11) . 2_655
U1 O1 U1 112.0(3) 2_655 .
U2 O1 U1 124.00(13) . .
U2 O1 U1 124.00(13) . 2_655
U1 O4 U1 109.9(3) . 2_655
C3 O5 U1 91.5(4) . 1_565
C3 O6 U1 95.3(4) . 1_565
C6 O7 U1 113.6(5) . .
C6 O8 U2 136.6(5) . .
C13 O9 U2 93.0(5) . .
N1 Cu1 N1 87.6(3) . 2_756
N2 Cu1 N1 91.1(2) . .
N2 Cu1 N1 176.4(2) 2_756 .
N2 Cu1 N1 91.1(2) 2_756 2_756
N2 Cu1 N1 176.4(2) . 2_756
N2 Cu1 N2 90.5(3) . 2_756
C3 U1 U1 129.96(15) 1_545 2_655
C3 U1 U2 168.09(15) 1_545 .
O1 U1 C3 163.9(2) . 1_545
O1 U1 O4 69.04(18) . .
O1 U1 O5 168.76(15) . 1_545
O1 U1 O6 139.45(17) . 1_545
O1 U1 O7 101.94(19) . .
O1 U1 U1 34.00(13) . 2_655
O1 U1 U2 27.92(13) . .
O2 U1 C3 91.9(2) . 1_545
O2 U1 O1 90.55(15) . .
O2 U1 O4 95.56(16) . .
O2 U1 O5 95.35(19) . 1_545
O2 U1 O6 84.1(2) . 1_545
O2 U1 O7 83.4(2) . .
O2 U1 U1 93.67(15) . 2_655
O2 U1 U2 87.80(15) . .
O3 U1 C3 85.3(2) . 1_545
O3 U1 O1 93.28(16) . .
O3 U1 O2 175.0(2) . .
O3 U1 O4 88.76(17) . .
O3 U1 O5 80.3(2) . 1_545
O3 U1 O6 95.0(2) . 1_545
O3 U1 O7 92.7(2) . .
O3 U1 U1 91.27(16) . 2_655
O3 U1 U2 94.11(16) . .
O4 U1 C3 94.9(2) . 1_545
O4 U1 O5 119.68(18) . 1_545
O4 U1 O6 71.53(17) . 1_545
O4 U1 O7 170.94(19) . .
O4 U1 U1 35.05(13) . 2_655
O4 U1 U2 96.96(13) . .
O5 U1 C3 25.62(18) 1_545 1_545
O5 U1 U1 154.10(12) 1_545 2_655
O5 U1 U2 142.59(12) 1_545 .
O6 U1 C3 25.60(18) 1_545 1_545
O6 U1 O5 51.03(16) 1_545 1_545
O6 U1 U1 106.11(12) 1_545 2_655
O6 U1 U2 165.13(12) 1_545 .
O7 U1 C3 94.1(2) . 1_545
O7 U1 O5 69.38(18) . 1_545
O7 U1 O6 117.19(18) . 1_545
O7 U1 U1 135.93(14) . 2_655
O7 U1 U2 74.03(14) . .
U1 U1 U2 61.912(5) 2_655 .
O1 U2 O8 77.93(14) . .
O1 U2 O8 77.93(14) . 2_655
O1 U2 O9 153.50(13) . .
O1 U2 O9 153.50(13) . 2_655
O1 U2 U1 28.088(5) . 2_655
O1 U2 U1 28.088(5) . .
O8 U2 O8 155.9(3) 2_655 .
O8 U2 O9 128.37(19) . .
O8 U2 O9 75.73(19) 2_655 .
O8 U2 O9 128.37(19) 2_655 2_655
O8 U2 O9 75.73(19) . 2_655
O8 U2 U1 103.91(13) 2_655 .
O8 U2 U1 52.46(14) . .
O8 U2 U1 103.91(13) . 2_655
O8 U2 U1 52.46(14) 2_655 2_655
O9 U2 O9 53.0(3) 2_655 .
O9 U2 U1 127.30(13) . 2_655
O9 U2 U1 166.67(17) 2_655 2_655
O9 U2 U1 127.30(13) 2_655 .
O9 U2 U1 166.67(17) . .
O10 U2 O1 91.22(17) 2_655 .
O10 U2 O1 91.22(17) . .
O10 U2 O8 86.4(2) 2_655 .
O10 U2 O8 94.1(2) . .
O10 U2 O8 94.1(2) 2_655 2_655
O10 U2 O8 86.4(2) . 2_655
O10 U2 O9 90.0(2) . .
O10 U2 O9 87.8(2) . 2_655
O10 U2 O9 87.8(2) 2_655 .
O10 U2 O9 90.0(2) 2_655 2_655
O10 U2 O10 177.6(3) . 2_655
O10 U2 U1 103.27(17) . .
O10 U2 U1 78.93(17) 2_655 .
O10 U2 U1 78.93(17) . 2_655
O10 U2 U1 103.27(17) 2_655 2_655
U1 U2 U1 56.176(11) 2_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C7 1.400(9) .
C1 N1 1.349(8) .
C2 C8 1.369(9) .
C2 N2 1.351(8) .
C3 C5 1.504(10) .
C3 O5 1.250(8) .
C3 O6 1.254(9) .
C3 U1 2.889(7) 1_565
C4 C6 1.516(9) .
C4 C8 1.417(10) .
C4 C14 1.380(10) .
C5 C7 1.398(10) .
C5 C11 1.398(10) .
C6 O7 1.235(9) .
C6 O8 1.276(9) .
C9 C14 1.386(10) .
C9 N2 1.349(8) .
C10 C11 1.389(10) .
C10 N1 1.363(9) .
C12 C13 1.503(14) .
C12 C15 1.393(10) .
C12 C15 1.393(10) 2_655
C13 O9 1.254(7) 2_655
C13 O9 1.254(7) .
C15 C16 1.402(11) .
C16 N3 1.353(10) .
N1 Cu1 2.037(6) .
N2 Cu1 2.034(5) .
N3 C16 1.353(10) 2_655
O1 U1 2.259(3) 2_655
O1 U1 2.259(3) .
O1 U2 2.247(6) .
O2 U1 1.799(5) .
O3 U1 1.776(5) .
O4 U1 2.288(4) .
O4 U1 2.288(4) 2_655
O5 U1 2.573(5) 1_565
O6 U1 2.490(5) 1_565
O7 U1 2.471(5) .
O8 U2 2.354(5) .
O9 U2 2.445(5) .
O10 U2 1.771(5) .
Cu1 N1 2.037(6) 2_756
Cu1 N2 2.034(5) 2_756
U1 C3 2.889(7) 1_545
U1 O5 2.573(5) 1_545
U1 O6 2.490(5) 1_545
U1 U1 3.7465(6) 2_655
U1 U2 3.9786(5) .
U2 O8 2.354(5) 2_655
U2 O9 2.444(5) 2_655
U2 O10 1.771(5) 2_655
U2 U1 3.9786(5) 2_655
