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_7247013
_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         'Nd, 2(C10 H8 N2 O2), 3(Au C2 N2), 5(H2 O)'
_chemical_formula_sum            'C26 H26 Au3 N10 Nd O9'
_chemical_formula_weight         1357.71
_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             2021-05-21
_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                89.082(4)
_cell_angle_beta                 85.457(4)
_cell_angle_gamma                70.612(2)
_cell_formula_units_Z            2
_cell_length_a                   7.9580(7)
_cell_length_b                   10.2731(10)
_cell_length_c                   23.067(2)
_cell_measurement_reflns_used    6642
_cell_measurement_temperature    190
_cell_measurement_theta_max      32.07
_cell_measurement_theta_min      2.27
_cell_volume                     1773.2(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2016)'
_computing_data_collection       'APEX-III v2019.1-0 (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2016)'
_computing_molecular_graphics
;
	Olex2 (Dolomanov et al., 2009) and ShelxLe (H\"ubschle, et al. 2021)
;
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'ShelXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      190
_diffrn_detector                 'Bruker CMOS PHOTON II area detector'
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_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_unetI/netI     0.0832
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9890
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.573
_diffrn_reflns_theta_min         1.771
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.874
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.5006
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 36745 reflections, Rint = 0.0605
 (14824 with I > 3sig(I), Rint = 0.0448)
;
_exptl_crystal_colour
;
	purple or colourless, depending on the light due to the Alexandrite Effect
;
_exptl_crystal_density_diffrn    2.543
_exptl_crystal_description       block
_exptl_crystal_F_000             1242
_exptl_crystal_preparation
;
	Allowed to evaporate until the crystals were JUST sticking out of the water.
	Almost, but not quite dry.
;
_exptl_crystal_recrystallization_method 'Slow evaporation from water'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.871
_refine_diff_density_min         -5.386
_refine_diff_density_rms         0.416
_refine_ls_extinction_coef       0.0011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL 2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         9890
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0633
_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^)+(0.1080P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1616
_refine_ls_wR_factor_ref         0.1775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7285
_reflns_number_total             9890
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00583f2.cif
_cod_data_source_block           NdWater5
_cod_depositor_comments
'Adding full bibliography for 7247008--7247022.cif.'
_cod_database_code               7247013
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.544
_shelx_estimated_absorpt_t_min   0.159
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8841(10)
 0.1159(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. 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
4. Rigid body (RIGU) restrains
 C15, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
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              51233
_shelx_hkl_checksum              98349
_olex2_date_sample_completion    2021-05-15
_olex2_date_sample_data_collection 2021-05-15
_olex2_date_sample_submission    2021-05-15
_olex2_exptl_crystal_mounting_method '150 um MiTiGen Micromount'