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_7247008
_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 Nd2 O12), 2(C2 H6 O)'
_chemical_formula_sum            'C30 H32 Au3 N10 Nd O8'
_chemical_formula_weight         1395.79
_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             2022-11-26
_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                 100.7180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9554(6)
_cell_length_b                   18.3762(10)
_cell_length_c                   19.9036(10)
_cell_measurement_reflns_used    4863
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.440
_cell_measurement_theta_min      2.216
_cell_volume                     3937.1(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 & ShelxLE'
_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 0.998
_diffrn_measured_fraction_theta_max 0.990
_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  0.0489
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15256
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.083
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.499
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0942 before and 0.0416 after correction. The Ratio of minimum to maximum transmission is 0.6908. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.355
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2572
_exptl_crystal_preparation
'Crystal was broken down to size, mounted directly from mother liqour'
_exptl_crystal_recrystallization_method
'Slow evaporation from 50:50 ethanol:water'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4855
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0182P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0562
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3370
_reflns_number_total             4855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00583f2.cif
_cod_data_source_block           NdEW
_cod_depositor_comments
'Adding full bibliography for 7247008--7247022.cif.'
_cod_database_code               7247008
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.574
_shelx_estimated_absorpt_t_min   0.225
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H13 of C13, H11 of C11, H10 of C10, H12 of C12, H16 of
  C16, H18 of C18, H17 of C17, H19 of C19
 At 1.5 times of:
  All C(H,H,H) groups, H2A of C21A, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C14-C15
 1.54 with sigma of 0.02
 H2B-N3
 2.17 with sigma of 0.02
 H2A-N3
 1.95 with sigma of 0.02
 O2A-H2A
 0.87 with sigma of 0.02
 O2B-H2B
 0.84 with sigma of 0.02
 C21A-H2A
 1.72 with sigma of 0.02
 C21B-H2B
 1.92 with sigma of 0.02
3. Others
 Sof(C21B)=Sof(H21C)=Sof(H21D)=Sof(C22B)=Sof(H22D)=Sof(H22E)=Sof(H22F)=
 Sof(O2B)=Sof(H2B)=1-FVAR(1)
 Sof(O2A)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C21A)=Sof(H21A)=
 Sof(H21B)=Sof(H2A)=FVAR(1)
4.a Rotating group:
 O1(H1A,H1B)
4.b Secondary CH2 refined with riding coordinates:
 C21A(H21A,H21B), C21B(H21C,H21D)
4.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C18(H18), C17(H17), C16(H16), C12(H12), C11(H11), C13(H13), C10(H10)
4.d Idealised Me refined as rotating group:
 C22A(H22A,H22B,H22C), C22B(H22D,H22E,H22F)
;
_shelx_res_checksum              52951
_shelx_hkl_checksum              44589
_olex2_date_sample_completion    2019-05-22
_olex2_date_sample_data_collection 2019-05-22
_olex2_date_sample_submission    2019-05-22
_olex2_exptl_crystal_mounting_method
'Duel-thickness MiTiGen Micrmount with parabar oil'
_olex2_submission_special_instructions 'No special instructions were received'