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_7042984
_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 (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 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       '\f and \w 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 \l/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/[\s^2^(Fo^2^)+(0.0207P)^2^+1.7454P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_cod_data_source_file            c7dt00942a2.cif
_cod_data_source_block           PPNchain12
_cod_database_code               7042984
_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_res_checksum              71638
_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'