#------------------------------------------------------------------------------
#$Date: 2017-05-18 05:28:16 +0300 (Thu, 18 May 2017) $
#$Revision: 196730 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/29/7042984.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_7042984
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         'Au C2 N4 O8 U, C36 H30 N P2'
_chemical_formula_sum            'C38 H30 Au N5 O8 P2 U'
_chemical_formula_weight         1181.60
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-30
_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                100.608(2)
_cell_angle_beta                 90.338(2)
_cell_angle_gamma                114.663(2)
_cell_formula_units_Z            1
_cell_length_a                   9.2421(3)
_cell_length_b                   10.8293(3)
_cell_length_c                   11.1451(2)
_cell_measurement_reflns_used    5930
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      69.52
_cell_measurement_theta_min      4.59
_cell_volume                     992.10(5)
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15618
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.385
_diffrn_reflns_theta_max         67.385
_diffrn_reflns_theta_min         4.053
_diffrn_source
'Microfocus sealed X-ray tub fitted with HELIOS multilayer optics'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    19.493
_exptl_absorpt_correction_T_max  0.7532
_exptl_absorpt_correction_T_min  0.5766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1455 before and 0.0670 after correction.
The Ratio of minimum to maximum transmission is 0.7655.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'dull yellow'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.978
_exptl_crystal_description       needle
_exptl_crystal_F_000             558
_exptl_crystal_preparation
'Slow evaporation from acetone: Acetone all evaporated.'
_exptl_crystal_recrystallization_method
'Slow evaporation from acetone: Acetone all evaporated.'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.058
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3487
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0337
_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)+(0.0207P)²+1.7454P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2484
_reflns_number_total             3487
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt00942a2.cif
_cod_data_source_block           PPNchain12
_cod_database_code               7042984
_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. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid body (RIGU) restrains
 C8, C9, C10, C11, C12, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2, O3, O4, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Au1, C1, N1, U1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_completion    2015-09-17
_olex2_date_sample_data_collection 2015-09-16
_olex2_date_sample_submission    2015-09-16
_olex2_exptl_crystal_mounting_method
'MiTeGen dual-thickness MicroMount using parabar oil'
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 0.0000 0.0000 0.5000 0.04425(15) Uani 1 2 d S TU P
Au1 Au 0.0000 0.0000 1.0000 0.05222(17) Uani 1 2 d S TU P
P1 P 1.1086(2) 0.5257(2) 0.11683(17) 0.0392(5) Uani 1 1 d . . .
O1 O 0.0996(8) -0.1065(6) 0.4677(5) 0.0644(17) Uani 1 1 d . . .
C1 C 0.0225(12) 0.0019(9) 0.8235(7) 0.060(2) Uani 1 1 d . U .
N1 N 0.0312(9) 0.0032(8) 0.7240(5) 0.064(2) Uani 1 1 d . U .
C3 C 0.9363(10) 0.3301(9) 0.2501(8) 0.054(2) Uani 1 1 d . . .
H3 H 0.9703 0.2713 0.1989 0.065 Uiso 1 1 calc R . .
N3 N 1.0000 0.5000 0.0000 0.059(3) Uani 1 2 d S T P
O3 O 0.4417(10) 0.3393(10) 0.5318(8) 0.111(3) Uani 1 1 d . U .
O2 O 0.2503(8) 0.1894(7) 0.6149(6) 0.0769(19) Uani 1 1 d . U .
C2 C 0.9919(9) 0.4675(7) 0.2398(6) 0.0411(19) Uani 1 1 d . . .
N2 N 0.3117(11) 0.2425(10) 0.5253(8) 0.075(2) Uani 1 1 d . U .
O4 O 0.2228(8) 0.1883(7) 0.4254(6) 0.0762(18) Uani 1 1 d . U .
C4 C 0.8318(11) 0.2795(12) 0.3347(10) 0.074(3) Uani 1 1 d . . .
H4 H 0.7927 0.1865 0.3394 0.089 Uiso 1 1 calc R . .
C5 C 0.7853(12) 0.3675(13) 0.4123(9) 0.075(3) Uani 1 1 d . . .
H5 H 0.7157 0.3336 0.4705 0.090 Uiso 1 1 calc R . .
C7 C 0.9447(10) 0.5565(9) 0.3190(7) 0.054(2) Uani 1 1 d . . .
H7 H 0.9823 0.6496 0.3145 0.064 Uiso 1 1 calc R . .
C6 C 0.8387(13) 0.5023(12) 0.4058(9) 0.074(3) Uani 1 1 d . . .
H6 H 0.8053 0.5599 0.4591 0.089 Uiso 1 1 calc R . .
C9 C 1.3524(12) 0.7581(10) 0.2622(9) 0.073(3) Uani 1 1 d . U .
H9 H 1.3636 0.6964 0.3054 0.087 Uiso 1 1 calc R . .
C8 C 1.2370(10) 0.7092(8) 0.1641(8) 0.0495(19) Uani 1 1 d . U .
C10 C 1.4497(14) 0.8965(11) 0.2957(13) 0.098(4) Uani 1 1 d . U .
H10 H 1.5291 0.9287 0.3602 0.117 Uiso 1 1 calc R . .
C11 C 1.4307(14) 0.9863(12) 0.2354(14) 0.111(4) Uani 1 1 d . U .
H11 H 1.4928 1.0811 0.2621 0.134 Uiso 1 1 calc R . .
C12 C 1.3242(15) 0.9415(11) 0.1378(15) 0.125(5) Uani 1 1 d . U .
H12 H 1.3159 1.0049 0.0953 0.150 Uiso 1 1 calc R . .
C13 C 1.2252(13) 0.8003(11) 0.0993(13) 0.097(4) Uani 1 1 d . U .
H13 H 1.1523 0.7688 0.0304 0.116 Uiso 1 1 calc R . .
C14 C 1.2333(9) 0.4338(7) 0.0910(7) 0.0405(17) Uani 1 1 d . . .
C15 C 1.3086(11) 0.4124(9) 0.1896(8) 0.062(2) Uani 1 1 d . . .
H15 H 1.2935 0.4439 0.2698 0.074 Uiso 1 1 calc R . .
C16 C 1.4050(12) 0.3443(10) 0.1662(11) 0.074(3) Uani 1 1 d . . .
H16 H 1.4549 0.3291 0.2310 0.089 Uiso 1 1 calc R . .
C17 C 1.4282(11) 0.2987(10) 0.0481(12) 0.072(3) Uani 1 1 d . . .
H17 H 1.4956 0.2545 0.0333 0.086 Uiso 1 1 calc R . .
C18 C 1.3549(12) 0.3173(9) -0.0458(10) 0.070(3) Uani 1 1 d . . .
H18 H 1.3708 0.2845 -0.1255 0.084 Uiso 1 1 calc R . .
C19 C 1.2559(10) 0.3840(8) -0.0273(8) 0.054(2) Uani 1 1 d . . .
H19 H 1.2049 0.3955 -0.0937 0.065 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -4.4197 7.2980 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 '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 U1 O1 180.0(2) 2_556 .
O1 U1 N1 89.6(2) 2_556 .
O1 U1 N1 90.4(2) . .
O1 U1 N1 89.6(2) . 2_556
O1 U1 N1 90.4(2) 2_556 2_556
O1 U1 O2 89.5(3) 2_556 2_556
O1 U1 O2 89.5(3) . .
O1 U1 O2 90.5(3) . 2_556
O1 U1 O2 90.5(3) 2_556 .
O1 U1 N2 91.5(3) . 2_556
O1 U1 N2 88.5(3) . .
O1 U1 N2 91.5(3) 2_556 .
O1 U1 N2 88.5(3) 2_556 2_556
O1 U1 O4 90.3(3) 2_556 .
O1 U1 O4 90.3(3) . 2_556
O1 U1 O4 89.7(3) 2_556 2_556
O1 U1 O4 89.7(3) . .
N1 U1 N1 180.0 . 2_556
N1 U1 N2 90.1(2) 2_556 .
N1 U1 N2 89.9(2) . .
N1 U1 N2 90.1(2) . 2_556
N1 U1 N2 89.9(2) 2_556 2_556
O2 U1 N1 115.3(2) 2_556 .
O2 U1 N1 64.7(2) . .
O2 U1 N1 64.7(2) 2_556 2_556
O2 U1 N1 115.3(2) . 2_556
O2 U1 O2 180.0 2_556 .
O2 U1 N2 25.2(2) 2_556 2_556
O2 U1 N2 154.8(2) 2_556 .
O2 U1 N2 154.8(2) . 2_556
O2 U1 N2 25.2(2) . .
N2 U1 N2 180.0 2_556 .
O4 U1 N1 115.1(2) . .
O4 U1 N1 64.9(2) 2_556 .
O4 U1 N1 64.9(2) . 2_556
O4 U1 N1 115.1(2) 2_556 2_556
O4 U1 O2 50.3(2) . .
O4 U1 O2 129.7(2) 2_556 .
O4 U1 O2 129.7(2) . 2_556
O4 U1 O2 50.3(2) 2_556 2_556
O4 U1 N2 154.8(2) 2_556 .
O4 U1 N2 25.2(2) . .
O4 U1 N2 25.2(2) 2_556 2_556
O4 U1 N2 154.8(2) . 2_556
O4 U1 O4 180.0 . 2_556
C1 Au1 C1 180.0 2_557 .
N3 P1 C2 111.1(3) . .
N3 P1 C8 109.7(3) . .
N3 P1 C14 111.7(3) . .
C2 P1 C8 108.9(4) . .
C2 P1 C14 107.1(3) . .
C14 P1 C8 108.3(3) . .
N1 C1 Au1 178.1(9) . .
C1 N1 U1 169.8(8) . .
C2 C3 H3 119.6 . .
C4 C3 H3 119.6 . .
C4 C3 C2 120.9(9) . .
P1 N3 P1 180.0 . 2_765
N2 O2 U1 97.7(6) . .
C3 C2 P1 119.9(6) . .
C3 C2 C7 119.5(7) . .
C7 C2 P1 120.3(6) . .
O3 N2 U1 177.3(8) . .
O3 N2 O2 124.6(10) . .
O3 N2 O4 121.3(9) . .
O2 N2 U1 57.1(5) . .
O2 N2 O4 114.1(9) . .
O4 N2 U1 57.1(5) . .
N2 O4 U1 97.7(6) . .
C3 C4 H4 120.3 . .
C3 C4 C5 119.4(10) . .
C5 C4 H4 120.3 . .
C4 C5 H5 119.4 . .
C6 C5 C4 121.2(9) . .
C6 C5 H5 119.4 . .
C2 C7 H7 120.8 . .
C2 C7 C6 118.4(9) . .
C6 C7 H7 120.8 . .
C5 C6 C7 120.6(9) . .
C5 C6 H6 119.7 . .
C7 C6 H6 119.7 . .
C8 C9 H9 119.9 . .
C10 C9 H9 119.9 . .
C10 C9 C8 120.2(10) . .
C9 C8 P1 120.9(7) . .
C13 C8 P1 119.9(8) . .
C13 C8 C9 119.2(9) . .
C9 C10 H10 120.0 . .
C11 C10 C9 120.0(12) . .
C11 C10 H10 120.0 . .
C10 C11 H11 119.5 . .
C12 C11 C10 121.0(11) . .
C12 C11 H11 119.5 . .
C11 C12 H12 119.8 . .
C11 C12 C13 120.4(11) . .
C13 C12 H12 119.8 . .
C8 C13 C12 119.0(11) . .
C8 C13 H13 120.5 . .
C12 C13 H13 120.5 . .
C15 C14 P1 120.9(6) . .
C19 C14 P1 119.9(6) . .
C19 C14 C15 119.2(7) . .
C14 C15 H15 120.4 . .
C16 C15 C14 119.2(9) . .
C16 C15 H15 120.4 . .
C15 C16 H16 119.8 . .
C17 C16 C15 120.4(10) . .
C17 C16 H16 119.8 . .
C16 C17 H17 119.8 . .
C18 C17 C16 120.5(9) . .
C18 C17 H17 119.8 . .
C17 C18 H18 119.3 . .
C17 C18 C19 121.4(9) . .
C19 C18 H18 119.3 . .
C14 C19 H19 120.3 . .
C18 C19 C14 119.3(9) . .
C18 C19 H19 120.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.745(6) 2_556
U1 O1 1.745(6) .
U1 N1 2.503(6) 2_556
U1 N1 2.503(6) .
U1 O2 2.497(7) 2_556
U1 O2 2.497(7) .
U1 N2 2.946(10) .
U1 N2 2.946(10) 2_556
U1 O4 2.496(6) .
U1 O4 2.496(6) 2_556
Au1 C1 1.983(8) 2_557
Au1 C1 1.983(8) .
P1 N3 1.549(2) .
P1 C2 1.791(7) .
P1 C8 1.809(8) .
P1 C14 1.805(7) .
C1 N1 1.115(10) .
C3 H3 0.9300 .
C3 C2 1.384(10) .
C3 C4 1.372(12) .
N3 P1 1.549(2) 2_765
O3 N2 1.212(11) .
O2 N2 1.263(10) .
C2 C7 1.393(10) .
N2 O4 1.267(10) .
C4 H4 0.9300 .
C4 C5 1.373(14) .
C5 H5 0.9300 .
C5 C6 1.348(14) .
C7 H7 0.9300 .
C7 C6 1.407(12) .
C6 H6 0.9300 .
C9 H9 0.9300 .
C9 C8 1.385(12) .
C9 C10 1.363(13) .
C8 C13 1.363(12) .
C10 H10 0.9300 .
C10 C11 1.346(15) .
C11 H11 0.9300 .
C11 C12 1.334(17) .
C12 H12 0.9300 .
C12 C13 1.395(14) .
C13 H13 0.9300 .
C14 C15 1.401(11) .
C14 C19 1.381(10) .
C15 H15 0.9300 .
C15 C16 1.373(12) .
C16 H16 0.9300 .
C16 C17 1.369(15) .
C17 H17 0.9300 .
C17 C18 1.334(14) .
C18 H18 0.9300 .
C18 C19 1.379(12) .
C19 H19 0.9300 .
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
U1 O2 N2 O3 -177.5(9)
U1 O2 N2 O4 4.5(9)
P1 C2 C7 C6 173.1(7)
P1 C8 C13 C12 179.4(10)
P1 C14 C15 C16 -178.8(7)
P1 C14 C19 C18 178.3(6)
C3 C2 C7 C6 -1.2(13)
C3 C4 C5 C6 1.0(16)
N3 P1 C2 C3 85.8(6)
N3 P1 C2 C7 -88.6(7)
N3 P1 C8 C9 -176.0(7)
N3 P1 C8 C13 1.1(9)
N3 P1 C14 C15 -163.1(6)
N3 P1 C14 C19 17.1(7)
O3 N2 O4 U1 177.5(9)
O2 N2 O4 U1 -4.5(9)
C2 P1 C8 C9 62.2(8)
C2 P1 C8 C13 -120.7(9)
C2 P1 C14 C15 -41.4(8)
C2 P1 C14 C19 138.9(6)
C2 C3 C4 C5 -1.8(14)
C2 C7 C6 C5 0.4(15)
C4 C3 C2 P1 -172.4(7)
C4 C3 C2 C7 1.9(13)
C4 C5 C6 C7 -0.3(16)
C9 C8 C13 C12 -3.4(17)
C9 C10 C11 C12 -4(2)
C8 P1 C2 C3 -153.4(6)
C8 P1 C2 C7 32.3(8)
C8 P1 C14 C15 76.0(8)
C8 P1 C14 C19 -103.8(7)
C8 C9 C10 C11 1.8(19)
C10 C9 C8 P1 179.1(9)
C10 C9 C8 C13 2.0(16)
C10 C11 C12 C13 3(2)
C11 C12 C13 C8 1(2)
C14 P1 C2 C3 -36.4(7)
C14 P1 C2 C7 149.2(7)
C14 P1 C8 C9 -53.9(8)
C14 P1 C8 C13 123.2(9)
C14 C15 C16 C17 0.5(15)
C15 C14 C19 C18 -1.5(12)
C15 C16 C17 C18 -1.4(16)
C16 C17 C18 C19 0.9(15)
C17 C18 C19 C14 0.6(13)
C19 C14 C15 C16 1.0(13)
