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_7247012
_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 H40 Au6 N20 O12 Sm0.81 Tb1.19), 4(H2 O)'
_chemical_formula_sum            'C26 H28 Au3 N10 O10 Sm0.41 Tb0.59'
_chemical_formula_weight         1386.93
_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                 91.485(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8699(7)
_cell_length_b                   19.2577(14)
_cell_length_c                   23.7813(17)
_cell_measurement_reflns_used    8690
_cell_measurement_temperature    230
_cell_measurement_theta_max      38.49
_cell_measurement_theta_min      2.28
_cell_volume                     3603.0(5)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40A (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      230
_diffrn_detector                 'Bruker CMOS PHOTON II area detector'
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker CMOS PHOTON II area detector'
_diffrn_measurement_method       '\f and \w 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  0.0475
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            28641
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.507
_diffrn_reflns_theta_min         1.713
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.046
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.4006
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1456 before and 0.0652 after correction. 
The Ratio of minimum to maximum transmission is 0.5356.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.557
_exptl_crystal_description       plate
_exptl_crystal_F_000             2539
_exptl_crystal_preparation
'crystal removed directly from the water and run before it could desolvate,Luminescent'
_exptl_crystal_recrystallization_method 'Crystallized from water'
_exptl_crystal_size_max          0.363
_exptl_crystal_size_mid          0.258
_exptl_crystal_size_min          0.136
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       0.00028(2)
_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   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         5509
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0144P)^2^+7.2450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0543
_refine_ls_wR_factor_ref         0.0564
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4815
_reflns_number_total             5509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00583f2.cif
_cod_data_source_block           2575SmTb6H2O
_cod_depositor_comments
'Adding full bibliography for 7247008--7247022.cif.'
_cod_database_code               7247012
_shelx_shelxl_version_number     2019/2
_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
 O2-H1B
 2 with sigma of 0.02
 O2-H3A
 3 with sigma of 0.02
 O1-H1B
 0.86 with sigma of 0.02
 O2-H2A = O2-H2B
 0.86 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Au2A) = Uanis(Au2B)
4. Others
 Sof(Sm1)=0.5*(1-FVAR(2))
 Sof(Tb1)=0.5*FVAR(2)
 Sof(Au2B)=0.5*(1-FVAR(3))
 Sof(Au2A)=0.5*FVAR(3)
 Fixed X: Au2A(1) Tb1(1) Sm1(1)
 Fixed Y: Au2A(0.5)
 Fixed Z: Au2A(0.5) Tb1(0.75) Sm1(0.75)
5.a Free rotating group:
 O3(H3A,H3B)
5.b 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              2739
_shelx_hkl_checksum              3040
_olex2_exptl_crystal_mounting_method 'Parabar oil on a MiTiGen'
_olex2_submission_special_instructions 'No special instructions were received'