Rapid and sensitive detection of vanillylmandelic acid based on a luminescent fourteen-metal Tb(III) planar nanocluster.
Meng, Yanheng; Wang, Shiqing; Lv, Xiaoli; Huang, Xianfeng; Zhang, Weibin; Wu, Xiaojun; Schipper, Desmond; Yang, Xiaoping; Chemical communications (Cambridge, England) 60 (2024) 14240–14243; doi:10.1039/d4cc03667k

data_7133965
_publ_section_title
;
 Rapid and sensitive detection of vanillylmandelic acid based on a
 luminescent fourteen-metal Tb(III) planar nanocluster.
;
_journal_issue                   96
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              14240
_journal_page_last               14243
_journal_paper_doi               10.1039/d4cc03667k
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C114 H146 N4 O82 Tb14, 4(H2 O)'
_chemical_formula_sum            'C114 H154 N4 O86 Tb14'
_chemical_formula_weight         5181.28
_chemical_name_systematic        cluster-1
_chemical_properties_physical    Heat-sensitive
_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     iterative
_audit_creation_date             2024-10-09
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6427)
;
_audit_update_record
;
2024-10-11 deposited with the CCDC.	2024-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.3630(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.4177(5)
_cell_length_b                   14.6058(3)
_cell_length_c                   43.1667(6)
_cell_measurement_reflns_used    83879
_cell_measurement_temperature    190.00
_cell_measurement_theta_max      30.0981
_cell_measurement_theta_min      1.2376
_cell_volume                     21063.4(6)
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      190.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0931
_diffrn_reflns_av_unetI/netI     0.0667
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            86704
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.798
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.707
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'DENZO and Scalepack (Otwinoski and Minor, 1997)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             9856
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.267
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     946
_refine_ls_number_reflns         18485
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+37.5237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14036
_reflns_number_total             18485
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03667k2.cif
_cod_data_source_block           d
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7133965.cif.
;
_cod_database_code               7133965
_shelx_shelxl_version_number     2014/7
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C35-C34
 1.55 with sigma of 0.002
 H43A-H41B_$1
 2.1 with sigma of 0.002
3. Others
 Fixed Y: O42(-0.28065)
4.a Riding coordinates:
 C45(H45A,H45B,H45C), O42(H42D,H42E), O43(H43A,H43B)
4.b Rotating group:
 O41(H41A,H41B)
4.c Ternary CH refined with riding coordinates:
 O14(H14), C33(H33)
4.d Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C34(H34A,H34B)
4.e Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C9(H9A,
 H9B,H9C), C11(H11A,H11B,H11C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C),
 C35(H35A,H35B,H35C), C42(H42A,H42B,H42C), C47(H47A,H47B,H47C), C48(H48A,H48B,
 H48C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C56(H56A,H56B,H56C), C57(H57A,
 H57B,H57C)
4.f Aromatic/amide H refined with riding coordinates:
 C14(H14A), C18(H18), C17(H17), C16(H16), C26(H26), C25(H25), C24(H24),
 C30(H30), C36(H36), C39(H39), C38(H38), C40(H40)
4.g Fitted hexagon refined as free rotating group:
 C15(C20,C19,C18,C17,C16), C28(C27,C26,C25,C24,C29), C39(C38,C37,C43,C41,C40)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              91897
_shelx_hkl_checksum              55844
_shelx_fab_checksum              48235
_olex2_submission_special_instructions 'No special instructions were received'