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_7247014
_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         'C26 H20 Au3 N10 O6 Sm0.78 Tb0.22, 3(H2 O)'
_chemical_formula_sum            'C26 H26 Au3 N10 O9 Sm0.79 Tb0.22'
_chemical_formula_weight         1365.66
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                89.150(2)
_cell_angle_beta                 85.419(2)
_cell_angle_gamma                70.588(2)
_cell_formula_units_Z            2
_cell_length_a                   7.8884(8)
_cell_length_b                   10.2453(10)
_cell_length_c                   23.058(2)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.210
_cell_measurement_theta_min      2.276
_cell_volume                     1751.8(3)
_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 0.912
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_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  0.0394
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            27111
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.343
_diffrn_reflns_theta_min         1.772
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.310
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.0851 before and 0.0391 after correction. 
The Ratio of minimum to maximum transmission is 0.7034. 
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.589
_exptl_crystal_description       prism
_exptl_crystal_F_000             1247
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'Slow evaporation from water'
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.094
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         8772
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0121P)^2^+3.1360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0434
_refine_ls_wR_factor_ref         0.0472
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6910
_reflns_number_total             8772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00583f2.cif
_cod_data_source_block           2575SmTb_5Water
_cod_depositor_comments
'Adding full bibliography for 7247008--7247022.cif.'
_cod_database_code               7247014
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.598
_shelx_estimated_absorpt_t_min   0.234
_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-H2B = O2-H2A
 0.9 with sigma of 0.02
 O3-H3A = O3-H3B = O4-H4A = O4-H4B
 0.9 with sigma of 0.02
 O5-H5A = O5-H5B
 0.9 with sigma of 0.02
 H1A-O5
 1.84 with sigma of 0.02
 H1B-O2
 1.86 with sigma of 0.02
 H2A-O3
 1.85 with sigma of 0.02
 H2B-N2_$1
 1.99 with sigma of 0.02
 H4B-O5_$2
 1.83 with sigma of 0.02
 H5A-N5_$1
 1.97 with sigma of 0.02
 H5B-N6_$3
 1.91 with sigma of 0.02
 H1A-H1B
 1.44 with sigma of 0.04
 H2A-H2B
 1.44 with sigma of 0.04
 H3A-H3B
 1.42 with sigma of 0.04
 H4A-H4B
 1.42 with sigma of 0.04
 H5A-H5B
 1.43 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(Sm1) = Uanis(Tb1)
4. Others
 Sof(Tb1)=1-FVAR(1)
 Sof(Sm1)=FVAR(1)
 Sof(Au2B)=0.5*(1-FVAR(3))
 Sof(Au2A)=0.5*FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26),
 C27(H27), C28(H28), C29(H29), C10(H10), C11(H11), C12(H12), C13(H13), C16(H16),
  C17(H17)
;
_shelx_res_checksum              56662
_shelx_hkl_checksum              43673
_olex2_date_sample_completion    2018-08-20
_olex2_date_sample_data_collection 2018-08-20
_olex2_date_sample_submission    2018-08-20
_olex2_exptl_crystal_mounting_method
'Parabar oil with MiTiGen Duel-thickeness MicroMounts'
_olex2_submission_special_instructions 'No special instructions were received'