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_7042987
_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 H26 Au2 N8 O6 U2'
_chemical_formula_sum            'C28 H26 Au2 N8 O6 U2'
_chemical_formula_weight         1440.57
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-02-15
_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                90
_cell_angle_beta                 109.867(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.4180(4)
_cell_length_b                   11.3951(3)
_cell_length_c                   12.7018(4)
_cell_measurement_reflns_used    6091
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      39.51
_cell_measurement_theta_min      2.47
_cell_volume                     1690.39(9)
_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, 2014)'
_computing_structure_solution
'XT (Version older then 2014/4) (Sheldrick, 2015)'
_diffrn_ambient_temperature      149.99
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.961
_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     0.0880
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12519
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         41.132
_diffrn_reflns_theta_min         1.982
_diffrn_source                   'Sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.255
_exptl_absorpt_correction_T_max  0.747914
_exptl_absorpt_correction_T_min  0.266999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
TWINABS-2012/1 (Bruker) was used for absorption correction.
wR2(int) was 0.1312 before and 0.1052 after correction.
HKLF 5 dataset constructed from all observations involving domain 2
Reflections merged according to point-group 2/m   
Single reflections that also occur in composites omitted
 Additional spherical absorption correction applied with mu*r =  0.2000
;
_exptl_crystal_colour            'dull light yellow'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.830
_exptl_crystal_description       prism
_exptl_crystal_F_000             1280
_exptl_crystal_preparation       'Solvothermal from MeCN'
_exptl_crystal_recrystallization_method 'Solvothermal from MeCN'
_exptl_crystal_size_max          0.299
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.123
_refine_diff_density_max         6.135
_refine_diff_density_min         -5.048
_refine_diff_density_rms         0.457
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         12519
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1008P)^2^+1.9259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1405
_refine_ls_wR_factor_ref         0.1634
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9618
_reflns_number_total             12519
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00942a2.cif
_cod_data_source_block           dimethylbipy
_cod_database_code               7042987
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5067(12) 0.4933(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O3-H3A
 1.02 with sigma of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C9(H9), C6(H6), C5(H5), C10(H10), C12(H12)
4.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              60764
_olex2_date_sample_completion    2015-01-25
_olex2_date_sample_data_collection 2015-01-25
_olex2_date_sample_submission    2015-01-24
_olex2_exptl_crystal_mounting_method
'MiTeGen dual-thickness MicroMount using parabar oil'