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_7247016
_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, 4(C2 H6 O)'
_chemical_formula_sum            'C60 H64 Au6 N20 O16 Sm Tb'
_chemical_formula_weight         2812.38
_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
_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                 99.557(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.8731(5)
_cell_length_b                   18.0339(9)
_cell_length_c                   19.5988(11)
_cell_measurement_reflns_used    9786
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.538
_cell_measurement_theta_min      2.493
_cell_volume                     3789.7(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 & ShelxLE'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator
'horizontally mounted graphite crystal (Triumph Monochromator, parallel)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            35573
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.561
_diffrn_reflns_theta_min         2.210
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.323
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4298
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1149 before and 0.0371 after correction. 
The Ratio of minimum to maximum transmission is 0.5761.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.465
_exptl_crystal_description       prism
_exptl_crystal_F_000             2586
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'Crystallized from 1:1 EtOH:H2O'
_exptl_crystal_size_max          0.457
_exptl_crystal_size_mid          0.369
_exptl_crystal_size_min          0.267
_refine_diff_density_max         1.485
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.000392(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         5789
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0178
_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^)+(0.0116P)^2^+14.0324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0366
_refine_ls_wR_factor_ref         0.0372
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5454
_reflns_number_total             5789
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00583f2.cif
_cod_data_source_block           SmTb11EW
_cod_depositor_comments
'Adding full bibliography for 7247008--7247022.cif.'
_cod_database_code               7247016
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.125
_shelx_estimated_absorpt_t_min   0.064
_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
2. Shared sites
{Sm1, Tb1}
3. Restrained distances
 H4B-O4 = H4A-O4
 0.9 with sigma of 0.02
 H4A-H4B
 1.37 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Sm1) = Uanis(Tb1)
5. Others
 Fixed Sof: Tb1(0.25) Sm1(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C14A(H14A,H14B)
6.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13)
6.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
;
_shelx_res_checksum              66532
_shelx_hkl_checksum              75803
_olex2_exptl_crystal_mounting_method
'Mounted with Parabar oil on a MiTiGen mount'