Selective fluoride sensing by a novel series of lanthanide-based one-dimensional coordination polymers through intramolecular proton transfer.
Singh, Vaibhav; Suresh, Lakshmi Thachanadan; Sutter, Jean-Pascal; Bar, Arun Kumar; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7436–7449; doi:10.1039/d4dt00598h

data_7715476
_publ_section_title
;
 Selective fluoride sensing by a novel series of lanthanide-based
 one-dimensional coordination polymers through intramolecular proton
 transfer.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7436
_journal_page_last               7449
_journal_paper_doi               10.1039/d4dt00598h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C41 H34 Dy N6 O8 P'
_chemical_formula_sum            'C41 H34 Dy N6 O8 P'
_chemical_formula_weight         932.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-19
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-02 deposited with the CCDC.	2024-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.806(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2035(4)
_cell_length_b                   14.9875(4)
_cell_length_c                   16.3982(4)
_cell_measurement_reflns_used    15654
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.9370
_cell_measurement_theta_min      3.0180
_cell_volume                     3831.73(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.816
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     19.00  45.00   0.50  282.77    --    7.10  38.00-112.00   52
  2  \w    -41.00 -16.00   0.50  282.77    --    7.10 -38.00  92.00   50
  3  \w    -56.00 -31.00   0.50  282.77    --   -7.50 -38.00  92.00   50
  4  \w     -8.00  17.00   0.50  282.77    --   -7.50  38.00-112.00   50
  5  \w     51.00  76.00   0.50  282.77    --    7.10  77.00 -60.00   50
  6  \w     61.00  90.00   0.50  282.77    --    7.10  77.00 150.00   58
  7  \w     50.00  93.00   0.50  282.77    --    7.10  77.00  60.00   86
  8  \w    -59.00  35.00   0.50  282.77    --   -7.50 -82.00  90.00  188
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0389576000
_diffrn_orient_matrix_UB_12      -0.0226360000
_diffrn_orient_matrix_UB_13      -0.0189065000
_diffrn_orient_matrix_UB_21      0.0080001000
_diffrn_orient_matrix_UB_22      0.0041034000
_diffrn_orient_matrix_UB_23      -0.0402453000
_diffrn_orient_matrix_UB_31      0.0221130000
_diffrn_orient_matrix_UB_32      -0.0413790000
_diffrn_orient_matrix_UB_33      0.0063680000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.816
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31126
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.816
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.957
_diffrn_reflns_theta_min         2.582
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.054
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic yellowish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       plate
_exptl_crystal_F_000             1868
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         8286
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0228
_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^)+(0.0273P)^2^+2.1066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0573
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7208
_reflns_number_total             8286
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00598h2.cif
_cod_data_source_block           aj1828
_cod_depositor_comments
'Adding full bibliography for 7715474--7715479.cif.'
_cod_database_code               7715476
_shelx_shelxl_version_number     2019/1
_chemical_oxdiff_formula         CHNODyP
_shelx_estimated_absorpt_t_max   0.821
_shelx_estimated_absorpt_t_min   0.762
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H37A,H37B} of C37, {H32,H32A} of C32, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H1A,H1B} of C1, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36)
\\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C33) \\sim Ueq: with sigma of 0.015 and sigma for terminal atoms of 0.03
Uanis(C37) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C36) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: H37A(0.5) H37B(0.5) H32(0.5) H32A(0.5) C33(0.5) H33(0.5) C35(0.5)
 H35(0.5) C34(0.5) H34(0.5) C36(0.5) H36(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B)
4.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C19(H19), C6(H6), C22(H22), C4(H4A), C20(H20), C5(H5), C31(H31),
 C29(H29), C21(H21), C43(H43), C16(H16), C13(H13), C32(H32), C32(H32A),
 C39(H39), C28(H28), C41(H41), C25(H25), C42(H42), C26(H26), C27(H27), C40(H40),
  C14(H14), C15(H15), C33(H33), C35(H35), C34(H34), C36(H36)
4.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
4.d Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_shelx_res_checksum              29348
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.376
_oxdiff_exptl_absorpt_empirical_full_min 0.803