Dicyanoaurate-based heterobimetallic uranyl coordination polymers.
Brown, Matthew L.; Ovens, Jeffrey S.; Leznoff, Daniel B.; Dalton transactions (Cambridge, England : 2003)  (2017) –; doi:10.1039/c7dt00942a

data_7042983
_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         'Au2 C4 N6 O12 U2, 2(C16 H36 N)'
_chemical_formula_sum            'C36 H72 Au2 N8 O12 U2'
_chemical_formula_weight         1679.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-13
_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                90
_cell_angle_beta                 94.481(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1927(18)
_cell_length_b                   32.757(6)
_cell_length_c                   14.629(2)
_cell_measurement_reflns_used    9273
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.588
_cell_measurement_theta_min      2.208
_cell_volume                     5347.2(15)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics
'Olex2 (Dolomanov et al., 2009), ShelXle (H\"ubschle et al., 2011)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution
'XT (of a version older than 2014/4)(Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0840
_diffrn_reflns_av_unetI/netI     0.1103
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43489
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.276
_diffrn_reflns_theta_min         1.870
_diffrn_source                   'Sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.565
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0836 before and 0.0562 after correction.
The Ratio of minimum to maximum transmission is 0.7161.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.086
_exptl_crystal_description       needle
_exptl_crystal_F_000             3128
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method
'The material was recrystallised from methanol by slow evaporation'
_exptl_crystal_size_max          0.452
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.027
_refine_diff_density_max         1.487
_refine_diff_density_min         -1.351
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         13816
_refine_ls_number_restraints     562
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1387
_refine_ls_R_factor_gt           0.0602
_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/[\s^2^(Fo^2^)+(0.0182P)^2^+13.0457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.1017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7441
_reflns_number_total             13816
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00942a2.cif
_cod_data_source_block           PeroxoMeOH
_cod_database_code               7042983
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C36-C37
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C28A) = Uanis(C28B)
Uanis(C29A) = Uanis(C29B)
Uanis(C16A) = Uanis(C16B)
Uanis(C19A) = Uanis(C19B)
Uanis(C21A) = Uanis(C21B)
4. 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
5. Others
 Sof(H18C)=Sof(H18D)=Sof(H20C)=Sof(H20D)=Sof(C19B)=Sof(H19C)=Sof(H19D)=
 Sof(C21B)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1)
 Sof(H18A)=Sof(H18B)=Sof(H20A)=Sof(H20B)=Sof(C19A)=Sof(H19A)=Sof(H19B)=
 Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(1)
 Sof(H27C)=Sof(H27D)=Sof(C28B)=Sof(H28C)=Sof(H28D)=Sof(C29B)=Sof(H29D)=
 Sof(H29E)=Sof(H29F)=1-FVAR(2)
 Sof(H27A)=Sof(H27B)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(C29A)=Sof(H29A)=
 Sof(H29B)=Sof(H29C)=FVAR(2)
 Sof(H15C)=Sof(H15D)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C16B)=Sof(H16C)=
 Sof(H16D)=1-FVAR(3)
 Sof(H15A)=Sof(H15B)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C16A)=Sof(H16A)=
 Sof(H16B)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B), C15(H15A,
 H15B), C15(H15C,H15D), C18(H18A,H18B), C18(H18C,H18D), C20(H20C,H20D),
 C20(H20A,H20B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,H26B),
  C27(H27A,H27B), C27(H27C,H27D), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,
 H32B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C38(H38A,H38B),
 C39(H39A,H39B), C40(H40A,H40B), C16A(H16A,H16B), C19A(H19A,H19B), C28A(H28A,
 H28B), C16B(H16C,H16D), C19B(H19C,H19D), C28B(H28C,H28D)
6.b Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C17(H17D,H17E,H17F)
6.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C25(H25A,H25B,H25C), C33(H33A,H33B,H33C), C37(H37A,H37B,
 H37C), C41(H41A,H41B,H41C), C21A(H21A,H21B,H21C), C29A(H29A,H29B,H29C),
 C21B(H21D,H21E,H21F), C29B(H29D,H29E,H29F)
;
_shelx_res_checksum              30574
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
;
The crystal was mounted on a MiTeGen dual-thickness MicroMounts 
    using parabar oil. 
The crystal was not centered well, so size should be considered approximate.'
;
_olex2_submission_special_instructions 'No special instructions were received'