Emissive lanthanide dicyanoaurate coordination polymers with 2,2′-bipyridine dioxide antenna groups and their hydration states
Brown, Matthew L.; Karpiuk, Thomas E.; Leznoff, Daniel B.; CrystEngComm 25 (2023) 4658–4668; doi:10.1039/D3CE00583F

data_7247011
_publ_section_title
;
 Emissive lanthanide dicyanoaurate coordination polymers with
 2,2&#x2032;-bipyridine dioxide antenna groups and their hydration states
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              4658
_journal_page_last               4668
_journal_paper_doi               10.1039/D3CE00583F
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety
;
0.5(C52 H32 Au6 Ce2 N20 O8), 2(C2 H6 O), 2(H2 O)
;
_chemical_formula_sum            'C30 H32 Au3 Ce N10 O8'
_chemical_formula_weight         1391.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-12-01 deposited with the CCDC.	2023-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.778(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.854(2)
_cell_length_b                   18.197(3)
_cell_length_c                   19.849(4)
_cell_measurement_reflns_used    9649
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.421
_cell_measurement_theta_min      2.208
_cell_volume                     3863.4(12)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics
;
Olex2 (Dolomanov et al., 2009) and ShelxLE (H\"ubschle et al., 2011)
;
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            39205
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.661
_diffrn_reflns_theta_min         2.082
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.571
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.4034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1441 before and 0.0509 after correction. 
The Ratio of minimum to maximum transmission is 0.5402.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.392
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2564
_exptl_crystal_recrystallization_method 'Slow evaporation from 1:1 EtOH:H2O'
_exptl_crystal_size_max          0.394
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.149
_refine_diff_density_min         -1.331
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         7375
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0253
_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^)+(0.0165P)^2^+11.9759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0496
_refine_ls_wR_factor_ref         0.0522
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6290
_reflns_number_total             7375
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00583f2.cif
_cod_data_source_block           CeEW
_cod_depositor_comments
'Adding full bibliography for 7247008--7247022.cif.'
_cod_original_cell_volume        3863.6(13)
_cod_database_code               7247011
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.188
_shelx_estimated_absorpt_t_min   0.083
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H,H,H) groups
2. Restrained distances
 O1-H1AA = O1-H1AB = O1-H1BC = O1-H1BD
 0.82 with sigma of 0.02
 H1BC-O2B
 1.86 with sigma of 0.02
 H1AA-H1AB
 1.31 with sigma of 0.04
 H1BC-H1BD
 1.31 with sigma of 0.04
3. Others
 Sof(H1BC)=Sof(H1BD)=Sof(O2B)=Sof(H2B)=Sof(C22B)=Sof(H22C)=Sof(H22D)=Sof(C23B)=
 Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(O2A)=Sof(H2A)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(C23A)=
 Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C22A(H22A,H22B), C22B(H22C,H22D)
4.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C19(H19), C18(H18), C17(H17), C16(H16), C13(H13)
4.c Idealised Me refined as rotating group:
 C23A(H23A,H23B,H23C), C23B(H23D,H23E,H23F)
4.d Idealised tetrahedral OH refined as rotating group:
 O2A(H2A), O2B(H2B)
;
_shelx_res_checksum              39288
_shelx_hkl_checksum              72742
_olex2_date_sample_data_collection 2019-04-17
_olex2_exptl_crystal_mounting_method 'MiTiGen Micromount'