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_7247009
_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         'C52 H40 Au6 N20 O12 Sm Tb, 8(H2 O)'
_chemical_formula_sum            'C52 H56 Au6 N20 O20 Sm Tb'
_chemical_formula_weight         2772.23
_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             2022-11-29
_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                 91.5120(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.8419(6)
_cell_length_b                   19.2528(15)
_cell_length_c                   23.7526(18)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.964
_cell_measurement_theta_min      2.283
_cell_volume                     3584.9(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 0.925
_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  0.0323
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            23074
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.213
_diffrn_reflns_theta_min         1.715
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.086
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.4699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1050 before and 0.0397 after correction. 
The Ratio of minimum to maximum transmission is 0.6297. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.568
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2538
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'Slow evaporation from water'
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.066
_refine_diff_density_max         2.570
_refine_diff_density_min         -1.569
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         5397
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0235P)^2^+36.8042P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0682
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4576
_reflns_number_total             5397
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00583f2.cif
_cod_data_source_block           5050SmTb6H2O
_cod_depositor_comments
'Adding full bibliography for 7247008--7247022.cif.'
_cod_database_code               7247009
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.457
_shelx_estimated_absorpt_t_min   0.119
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O1-H1A = O1-H1B = O2_$1-H2A_$1 = O2_$1-H2B_$1 = O3_$1-H3A_$1 = O3_$1-H3B_$1
 0.9 with sigma of 0.02
 H2A-H3B
 2.2 with sigma of 0.02
 O2-H1A
 1.82 with sigma of 0.02
 H1A-H1B
 1.424 with sigma of 0.04
 H2A-H2B
 1.409 with sigma of 0.04
 H3A-H3B
 1.423 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Au2A \\sim Au2B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(Tb1) = Uanis(Sm1)
4. Rigid body (RIGU) restrains
 Au2A, Au2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Au2B)=0.5*(1-FVAR(2))
 Sof(Au2A)=0.5*FVAR(2)
 Fixed Sof: Sm1(0.25) Tb1(0.25)
6.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C16(H16), C17(H17), C18(H18), C19(H19)
;
_shelx_res_checksum              71936
_shelx_hkl_checksum              40326
_olex2_date_sample_completion    2018-08-17
_olex2_date_sample_data_collection 2018-08-17
_olex2_date_sample_submission    2018-08-17
_olex2_exptl_crystal_mounting_method
'Parabar oil on a MiTiGen Duel-Thickness micromount'