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_7042982
_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      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
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-03-14 deposited with the CCDC.
2017-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                88.081(5)
_cell_angle_beta                 86.958(5)
_cell_angle_gamma                89.110(5)
_cell_formula_units_Z            4
_cell_length_a                   11.231(2)
_cell_length_b                   15.587(3)
_cell_length_c                   29.978(6)
_cell_measurement_reflns_used    9852
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.561
_cell_measurement_theta_min      2.252
_cell_volume                     5237.0(17)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.865
_diffrn_measured_fraction_theta_max 0.688
_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_unetI/netI     0.1075
_diffrn_reflns_Laue_measured_fraction_full 0.865
_diffrn_reflns_Laue_measured_fraction_max 0.688
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18412
_diffrn_reflns_point_group_measured_fraction_full 0.865
_diffrn_reflns_point_group_measured_fraction_max 0.688
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.328
_diffrn_reflns_theta_min         1.307
_diffrn_source                   'Sealed tube'
_exptl_absorpt_coefficient_mu    11.809
_exptl_absorpt_correction_T_max  0.745708
_exptl_absorpt_correction_T_min  0.512661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
TWINABS-2012/1 (Bruker) was used for absorption correction.
wR2(int) was 0.0784 before and 0.0611 after correction.
The Ratio of minimum to maximum transmission is 0.7161. 
Additional spherical absorption correction applied with mu*r =  0.2000
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.130
_exptl_crystal_description       prism
_exptl_crystal_F_000             3128
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method
'The material was crystallised from ethanol by slow evaporation'
_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.024
_refine_diff_density_max         3.963
_refine_diff_density_min         -2.121
_refine_diff_density_rms         0.305
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1136
_refine_ls_number_reflns         18412
_refine_ls_number_restraints     1164
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1536
_refine_ls_R_factor_gt           0.0841
_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^)+(0.0448P)^2^+336.3640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1754
_refine_ls_wR_factor_ref         0.2006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10658
_reflns_number_total             18412
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00942a2.cif
_cod_data_source_block           PeroxoEtOH
_cod_original_cell_volume        5236.9(17)
_cod_database_code               7042982
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.249
_shelx_estimated_absorpt_t_max   0.765
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.505(11) 0.495(11)
2. 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
3. Restrained distances
 C43-C44A
 1.5 with sigma of 0.02
 C43-C44B
 1.5 with sigma of 0.02
 C44A-C45A
 1.5 with sigma of 0.02
 C44B-C45B
 1.5 with sigma of 0.02
 C43-C45A
 2.54 with sigma of 0.02
 C43-C45B
 2.54 with sigma of 0.02
 C52B-C53B
 1.5 with sigma of 0.02
 C52A-C52B
 1.5 with sigma of 0.02
 C51B-C53B
 2.54 with sigma of 0.02
 C51A-C53A
 2.54 with sigma of 0.02
 C36-C37A \\sim C36-C37B
 with sigma of 0.02
 C50-C51A \\sim C50-C51B
 with sigma of 0.02
 C51A-C52A \\sim C51B-C52B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C4 \\sim N4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C44A \\sim C44B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C37A \\sim C37B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C45A \\sim C45B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C51A \\sim C51B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C52A \\sim C52B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(O2) = Uanis(O1)
Uanis(O4) = Uanis(O3)
Uanis(C53A) = Uanis(C53B)
5. 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
6. Others
 Sof(H43C)=Sof(H43D)=Sof(C44B)=Sof(H44C)=Sof(H44D)=Sof(C45B)=Sof(H45D)=
 Sof(H45E)=Sof(H45F)=1-FVAR(1)
 Sof(H43A)=Sof(H43B)=Sof(C44A)=Sof(H44A)=Sof(H44B)=Sof(C45A)=Sof(H45A)=
 Sof(H45B)=Sof(H45C)=FVAR(1)
 Sof(H50C)=Sof(H50D)=Sof(C51B)=Sof(H51C)=Sof(H51D)=Sof(C52B)=Sof(H52C)=
 Sof(H52D)=Sof(C53B)=Sof(H53D)=Sof(H53E)=Sof(H53F)=1-FVAR(2)
 Sof(H50A)=Sof(H50B)=Sof(C51A)=Sof(H51A)=Sof(H51B)=Sof(C52A)=Sof(H52A)=
 Sof(H52B)=Sof(C53A)=Sof(H53A)=Sof(H53B)=Sof(H53C)=FVAR(2)
 Sof(H36C)=Sof(H36D)=Sof(C37B)=Sof(H37D)=Sof(H37E)=Sof(H37F)=1-FVAR(3)
 Sof(H36A)=Sof(H36B)=Sof(C37A)=Sof(H37A)=Sof(H37B)=Sof(H37C)=FVAR(3)
7.a Secondary CH2 refined with riding coordinates:
 C01M(H01C,H01D), C01V(H01A,H01B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,
 H26B), C27(H27A,H27B), C28(H28A,H28B), C30(H30A,H30B), C31(H31A,H31B),
 C32(H32A,H32B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C36(H36C,H36D),
  C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C42(H42A,H42B), C43(H43A,
 H43B), C43(H43C,H43D), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B),
 C50(H50A,H50B), C50(H50C,H50D), C55(H55A,H55B), C56(H56A,H56B), C58(H58A,H58B),
  C59(H59A,H59B), C60(H60A,H60B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,
 H64B), C66(H66A,H66B), C67(H67A,H67B), C69(H69A,H69B), C70(H70A,H70B),
 C71(H71A,H71B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C77(H77A,H77B),
  C78(H78A,H78B), C79(H79A,H79B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,
 H83B), C54(H54A,H54B), C44A(H44A,H44B), C44B(H44C,H44D), C51A(H51A,H51B),
 C52A(H52A,H52B), C51B(H51C,H51D), C52B(H52C,H52D)
7.b Me refined with riding coordinates:
 C37A(H37A,H37B,H37C), C37B(H37D,H37E,H37F), C45A(H45A,H45B,H45C), C45B(H45D,
 H45E,H45F)
7.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C29(H29A,H29B,H29C), C33(H33A,H33B,H33C), C41(H41A,H41B,
 H41C), C57(H57A,H57B,H57C), C61(H61A,H61B,H61C), C65(H65A,H65B,H65C), C68(H68A,
 H68B,H68C), C72(H72A,H72B,H72C), C76(H76A,H76B,H76C), C80(H80A,H80B,H80C),
 C84(H84A,H84B,H84C), C49(H49A,H49B,H49C), C53A(H53A,H53B,H53C), C53B(H53D,H53E,
 H53F)
;
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN using parabar oil'
_shelx_res_checksum              31713