#------------------------------------------------------------------------------
#$Date: 2017-05-18 05:28:16 +0300 (Thu, 18 May 2017) $
#$Revision: 196730 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/29/7042990.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_7042990
loop_
_publ_author_name
'Brown, Matthew L.'
'Ovens, Jeffrey S.'
'Leznoff, Daniel B.'
_publ_section_title
;
 Dicyanoaurate-based heterobimetallic uranyl coordination polymers.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/c7dt00942a
_journal_year                    2017
_chemical_formula_moiety         'C28 H30 Au2 N8 O8 U2'
_chemical_formula_sum            'C28 H30 Au2 N8 O8 U2'
_chemical_formula_weight         1476.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-07-07
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-03-14 deposited with the CCDC.
2017-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                113.603(4)
_cell_angle_beta                 97.039(4)
_cell_angle_gamma                99.801(4)
_cell_formula_units_Z            1
_cell_length_a                   6.1056(9)
_cell_length_b                   12.5052(18)
_cell_length_c                   13.1277(19)
_cell_measurement_reflns_used    4105
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.05
_cell_measurement_theta_min      3.01
_cell_volume                     884.7(2)
_computing_molecular_graphics
'Olex2 (Dolomanov et al., 2009), ShelXle (Hübschle et al., 2011)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution
'XT (Version older then 2014/4) (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0762
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9477
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.443
_diffrn_reflns_theta_min         1.831
_diffrn_source                   'Sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.448
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0712 before and 0.0469 after correction.
The Ratio of minimum to maximum transmission is 0.7971.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.772
_exptl_crystal_description       needle
_exptl_crystal_F_000             660
_exptl_crystal_preparation
'No video taken, cannot determine crystal size.'
_exptl_crystal_recrystallization_method
'The material was crystallised from methanol by slow evaporation'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.015
_refine_diff_density_max         2.872
_refine_diff_density_min         -1.660
_refine_diff_density_rms         0.247
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3261
_refine_ls_number_restraints     225
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0488
_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)+(0.0313P)²+1.7779P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0833
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2339
_reflns_number_total             3261
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt00942a2.cif
_cod_data_source_block           bipyChain
_cod_original_cell_volume        884.6(2)
_cod_database_code               7042990
_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.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9895(14) 0.0105(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C11(H11)
4.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_completion    2014-05-13
_olex2_date_sample_data_collection 2014-05-12
_olex2_date_sample_submission    2014-05-07
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'MiTeGen dual-thickness MicroMount using parabar oil'
_olex2_submission_original_sample_id MLB83
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-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
U1 U 0.78372(8) 0.75846(4) 0.52495(3) 0.02590(14) Uani 1 1 d . U .
H4 H 0.343(16) 0.769(9) 0.580(8) 0.01(3) Uiso 1 1 d . . .
Au1 Au 1.0000 1.0000 1.0000 0.0366(2) Uani 1 2 d S U P
Au2 Au 0.5000 1.0000 1.0000 0.0478(2) Uani 1 2 d S U P
O2 O 0.7113(13) 0.8886(7) 0.5278(6) 0.0386(19) Uani 1 1 d . U .
O3 O 0.8458(13) 0.6246(8) 0.5180(7) 0.043(2) Uani 1 1 d . U .
O4 O 0.4393(13) 0.7221(8) 0.5870(7) 0.037(2) Uani 1 1 d . U .
O5 O 1.1548(12) 0.8428(7) 0.5779(6) 0.0353(19) Uani 1 1 d . U .
N1 N 0.8747(16) 0.8507(10) 0.7375(8) 0.046(3) Uani 1 1 d . U .
N2 N 0.357(2) 0.7318(12) 0.9614(11) 0.064(3) Uani 1 1 d . U .
N3 N 0.4765(14) 0.6227(8) 0.3383(7) 0.027(2) Uani 1 1 d . U .
N4 N 0.8881(14) 0.7422(8) 0.3332(7) 0.0264(19) Uani 1 1 d . U .
C1 C 0.921(2) 0.9048(12) 0.8337(10) 0.043(3) Uani 1 1 d . U .
C2 C 0.413(2) 0.8305(15) 0.9770(12) 0.051(3) Uani 1 1 d . U .
C3 C 1.267(2) 0.9661(11) 0.6453(12) 0.049(3) Uani 1 1 d . U .
H3A H 1.3467 0.9978 0.5990 0.073 Uiso 1 1 calc R U .
H3B H 1.3775 0.9734 0.7100 0.073 Uiso 1 1 calc R U .
H3C H 1.1551 1.0120 0.6732 0.073 Uiso 1 1 calc R U .
C14 C 1.089(2) 0.8029(10) 0.3312(10) 0.036(3) Uani 1 1 d . U .
H14 H 1.2075 0.8349 0.3973 0.043 Uiso 1 1 calc R U .
C4 C 0.387(2) 0.6754(13) 0.6658(11) 0.052(4) Uani 1 1 d . U .
H4A H 0.2985 0.5917 0.6244 0.077 Uiso 1 1 calc R U .
H4B H 0.2971 0.7234 0.7147 0.077 Uiso 1 1 calc R U .
H4C H 0.5278 0.6788 0.7127 0.077 Uiso 1 1 calc R U .
C5 C 0.288(2) 0.5525(11) 0.3398(11) 0.040(3) Uani 1 1 d . U .
H5 H 0.2696 0.5501 0.4098 0.048 Uiso 1 1 calc R U .
C6 C 0.118(2) 0.4829(12) 0.2443(11) 0.047(3) Uani 1 1 d . U .
H6 H -0.0140 0.4337 0.2484 0.056 Uiso 1 1 calc R U .
C7 C 0.144(2) 0.4862(12) 0.1453(11) 0.050(3) Uani 1 1 d . U .
H7 H 0.0282 0.4401 0.0788 0.060 Uiso 1 1 calc R U .
C8 C 0.337(2) 0.5555(11) 0.1401(10) 0.044(3) Uani 1 1 d . U .
H8 H 0.3559 0.5578 0.0702 0.053 Uiso 1 1 calc R U .
C12 C 0.967(2) 0.7788(11) 0.1454(10) 0.043(3) Uani 1 1 d . U .
H12 H 0.9918 0.7932 0.0815 0.052 Uiso 1 1 calc R U .
C9 C 0.5056(18) 0.6228(10) 0.2379(9) 0.029(2) Uani 1 1 d . U .
C13 C 1.134(2) 0.8213(11) 0.2393(10) 0.045(3) Uani 1 1 d . U .
H13 H 1.2806 0.8635 0.2413 0.054 Uiso 1 1 calc R U .
C10 C 0.7207(18) 0.6941(10) 0.2364(9) 0.026(2) Uani 1 1 d . U .
C11 C 0.760(2) 0.7141(11) 0.1445(10) 0.040(3) Uani 1 1 d . U .
H11 H 0.6418 0.6827 0.0786 0.048 Uiso 1 1 calc R 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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 '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'
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
O2 U1 O3 177.6(4) . .
O2 U1 O5 93.7(3) . .
O3 U1 O5 88.5(3) . .
O2 U1 O4 85.9(3) . .
O3 U1 O4 92.9(3) . .
O5 U1 O4 145.9(3) . .
O2 U1 N1 90.2(4) . .
O3 U1 N1 91.4(4) . .
O5 U1 N1 73.8(3) . .
O4 U1 N1 72.1(3) . .
O2 U1 N4 82.4(3) . .
O3 U1 N4 97.1(3) . .
O5 U1 N4 78.0(3) . .
O4 U1 N4 135.3(3) . .
N1 U1 N4 150.3(3) . .
O2 U1 N3 91.7(3) . .
O3 U1 N3 86.0(3) . .
O5 U1 N3 139.1(3) . .
O4 U1 N3 74.9(3) . .
N1 U1 N3 146.7(3) . .
N4 U1 N3 62.7(3) . .
C1 Au1 C1 180.0 2_777 .
C1 Au1 Au2 90.4(4) 2_777 .
C1 Au1 Au2 89.6(4) . .
C1 Au1 Au2 89.6(4) 2_777 1_655
C1 Au1 Au2 90.4(4) . 1_655
Au2 Au1 Au2 180.0 . 1_655
C2 Au2 C2 180.0 2_677 .
C2 Au2 Au1 86.2(4) 2_677 .
C2 Au2 Au1 93.8(4) . .
C2 Au2 Au1 93.8(4) 2_677 1_455
C2 Au2 Au1 86.2(4) . 1_455
Au1 Au2 Au1 180.0 . 1_455
C4 O4 U1 131.2(7) . .
C4 O4 O5 105.9(7) . 1_455
U1 O4 O5 119.0(4) . 1_455
C4 O4 H4 111(6) . .
U1 O4 H4 114(6) . .
O5 O4 H4 5(6) 1_455 .
C3 O5 U1 128.5(7) . .
C1 N1 U1 172.3(12) . .
C5 N3 C9 118.4(10) . .
C5 N3 U1 121.1(7) . .
C9 N3 U1 120.6(7) . .
C14 N4 C10 117.7(10) . .
C14 N4 U1 120.9(7) . .
C10 N4 U1 119.7(7) . .
N1 C1 Au1 179.4(13) . .
N2 C2 Au2 177.8(13) . .
O5 C3 H3A 109.5 . .
O5 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
O5 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
N4 C14 C13 123.5(12) . .
N4 C14 H14 118.3 . .
C13 C14 H14 118.3 . .
O4 C4 H4A 109.5 . .
O4 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
O4 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
N3 C5 C6 122.9(12) . .
N3 C5 H5 118.6 . .
C6 C5 H5 118.6 . .
C7 C6 C5 118.6(13) . .
C7 C6 H6 120.7 . .
C5 C6 H6 120.7 . .
C6 C7 C8 120.1(12) . .
C6 C7 H7 120.0 . .
C8 C7 H7 120.0 . .
C7 C8 C9 119.5(12) . .
C7 C8 H8 120.2 . .
C9 C8 H8 120.2 . .
C13 C12 C11 118.5(12) . .
C13 C12 H12 120.8 . .
C11 C12 H12 120.8 . .
N3 C9 C8 120.4(11) . .
N3 C9 C10 117.6(9) . .
C8 C9 C10 121.9(11) . .
C12 C13 C14 119.2(12) . .
C12 C13 H13 120.4 . .
C14 C13 H13 120.4 . .
C11 C10 N4 119.7(11) . .
C11 C10 C9 123.3(10) . .
N4 C10 C9 117.0(10) . .
C10 C11 C12 121.4(12) . .
C10 C11 H11 119.3 . .
C12 C11 H11 119.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O2 1.745(8) .
U1 O3 1.748(8) .
U1 O5 2.223(7) .
U1 O4 2.384(8) .
U1 N1 2.500(10) .
U1 N4 2.610(9) .
U1 N3 2.620(9) .
Au1 C1 1.970(12) 2_777
Au1 C1 1.970(12) .
Au1 Au2 3.0528(5) .
Au1 Au2 3.0528(5) 1_655
Au2 C2 1.982(17) 2_677
Au2 C2 1.982(17) .
Au2 Au1 3.0528(5) 1_455
O4 C4 1.420(14) .
O4 O5 2.509(11) 1_455
O4 H4 0.92(9) .
O5 C3 1.425(14) .
N1 C1 1.137(14) .
N2 C2 1.149(17) .
N3 C5 1.331(14) .
N3 C9 1.352(13) .
N4 C14 1.339(14) .
N4 C10 1.372(13) .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C14 C13 1.366(16) .
C14 H14 0.9500 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 C6 1.380(16) .
C5 H5 0.9500 .
C6 C7 1.344(17) .
C6 H6 0.9500 .
C7 C8 1.364(17) .
C7 H7 0.9500 .
C8 C9 1.390(15) .
C8 H8 0.9500 .
C12 C13 1.350(16) .
C12 C11 1.376(17) .
C12 H12 0.9500 .
C9 C10 1.464(16) .
C13 H13 0.9500 .
C10 C11 1.366(15) .
C11 H11 0.9500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C10 N4 C14 C13 1.5(16)
U1 N4 C14 C13 -163.9(9)
C9 N3 C5 C6 -2.2(17)
U1 N3 C5 C6 177.6(9)
N3 C5 C6 C7 0(2)
C5 C6 C7 C8 1(2)
C6 C7 C8 C9 0(2)
C5 N3 C9 C8 3.2(16)
U1 N3 C9 C8 -176.6(8)
C5 N3 C9 C10 -175.8(10)
U1 N3 C9 C10 4.3(13)
C7 C8 C9 N3 -2.1(18)
C7 C8 C9 C10 176.9(12)
C11 C12 C13 C14 -2.5(18)
N4 C14 C13 C12 1.3(19)
C14 N4 C10 C11 -3.1(15)
U1 N4 C10 C11 162.5(8)
C14 N4 C10 C9 176.9(10)
U1 N4 C10 C9 -17.5(12)
N3 C9 C10 C11 -171.4(11)
C8 C9 C10 C11 9.6(17)
N3 C9 C10 N4 8.6(14)
C8 C9 C10 N4 -170.4(10)
N4 C10 C11 C12 2.0(17)
C9 C10 C11 C12 -178.1(11)
C13 C12 C11 C10 0.9(19)
C1 Au1 Au2 C2 75.1(6)
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.9895(14)
2 0.0105(14)
