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_7042986
_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         'C36 H30 N2 P2, C2 N2 O6 Au U'
_chemical_formula_sum            'C38 H30 Au N4 O6 P2 U'
_chemical_formula_weight         1135.59
_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   difmap
_audit_creation_date             2017-02-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-03-14 deposited with the CCDC.
2017-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                69.826(2)
_cell_angle_beta                 77.625(2)
_cell_angle_gamma                84.510(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1439(5)
_cell_length_b                   12.7533(6)
_cell_length_c                   15.0713(8)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.012
_cell_measurement_theta_min      2.381
_cell_volume                     1963.28(17)
_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-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.915
_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     0.0657
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12930
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.615
_diffrn_reflns_theta_min         1.467
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    7.981
_exptl_absorpt_correction_T_max  0.746432
_exptl_absorpt_correction_T_min  0.468435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_description       prism
_exptl_crystal_F_000             1070
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method 'Slow evaporation from methanol'
_exptl_crystal_size_max          0.483
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.069
_refine_diff_density_min         -2.208
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         12930
_refine_ls_number_restraints     554
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0233P)^2^+11.1391P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10285
_reflns_number_total             12930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00942a2.cif
_cod_data_source_block           PPNPeroxo
_cod_database_code               7042986
_shelx_shelxl_version_number     2016/6
_exptl_absorpt_special_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1020 before and 0.0716 after correction.
 The Ratio of minimum to maximum transmission is 0.63.
  The \l/2 correction factor is Not present

Final HKLF 4 output contains 96472 reflections, Rint = 0.0642
 (34228 with I > 3sig(I), Rint = 0.0401) (HKLF 5 used)
 
 HKLF 5 dataset constructed from all observations involving domain 1
   25633 Corrected reflections written to file twin5.hkl
 Reflections merged according to point-group -1    
 Single reflections that also occur in composites omitted
  Additional spherical absorption correction applied with mu*r =  0.2000
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder with Parabar oil'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7522(6) 0.2478(6)
2. Restrained distances
 C4-H4
 0.95 with sigma of 0.02
 C5-H5
 0.95 with sigma of 0.02
 C6-H6
 0.95 with sigma of 0.02
 C7-H7
 0.95 with sigma of 0.02
 C8-H8
 0.95 with sigma of 0.02
 C10-H10
 0.95 with sigma of 0.02
 C11-H11
 0.95 with sigma of 0.02
 C12-H12
 0.95 with sigma of 0.02
 C13-H13
 0.95 with sigma of 0.02
 C14-H14
 0.95 with sigma of 0.02
 C16-H16
 0.95 with sigma of 0.02
 C17-H17
 0.95 with sigma of 0.02
 C18-H18
 0.95 with sigma of 0.02
 C19-H19
 0.95 with sigma of 0.02
 C20-H20
 0.95 with sigma of 0.02
 C22-H22
 0.95 with sigma of 0.02
 C23-H23
 0.95 with sigma of 0.02
 C24-H24
 0.95 with sigma of 0.02
 C25-H25
 0.95 with sigma of 0.02
 C26-H26
 0.95 with sigma of 0.02
 C28-H28
 0.95 with sigma of 0.02
 C29-H29
 0.95 with sigma of 0.02
 C30-H30
 0.95 with sigma of 0.02
 C31-H31
 0.95 with sigma of 0.02
 C32-H32
 0.95 with sigma of 0.02
 C34-H34
 0.95 with sigma of 0.02
 C35-H35
 0.95 with sigma of 0.02
 C36-H36
 0.95 with sigma of 0.02
 C37-H37
 0.95 with sigma of 0.02
 C38-H38
 0.95 with sigma of 0.02
 U1-O4B \\sim U1-O4A
 with sigma of 0.02
 U1-O6B \\sim U1-O6A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O5B \\sim O5A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.01
O4B \\sim O4A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O6B \\sim O6A: within 2A with sigma of 0.03 and sigma for terminal atoms of 0.06
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
 Fixed Sof: O3A(0.5) O2A(0.5) O4A(0.5) O6A(0.5) O5A(0.5) N3B(0.5) O3B(0.5)
 O2B(0.5) O4B(0.5) O6B(0.5) O5B(0.5) N3A(0.5) O1A(0.5) O1B(0.5)
;
_shelx_res_checksum              52301