Intercalation of a manganese(ii)-thiacalixarene luminescent complex in layered double hydroxides: synthesis and photophysical characterization
O’Toole, Niall; Lecourt, Constance; Suffren, Yan; Toche, François; Chiriac, Rodica; Gilon, Nicole; Bessueille, François; Brioude, Arnaud; Jeanneau, Erwann; Luneau, Dominique; Desroches, Cédric; New Journal of Chemistry 45 (2021) 343–350; doi:10.1039/D0NJ04890A

data_7060152
_publ_section_title
;
 Intercalation of a manganese(ii)-thiacalixarene luminescent complex in
 layered double hydroxides: synthesis and photophysical characterization
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              343
_journal_page_last               350
_journal_paper_doi               10.1039/D0NJ04890A
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C92 H120 Al4 N4 O32 S8'
_chemical_formula_sum            'C92 H120 Al4 N4 O32 S8'
_chemical_formula_weight         2158.31
_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             2020-06-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-06-15 deposited with the CCDC.	2020-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.421(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9486(4)
_cell_length_b                   22.9133(7)
_cell_length_c                   20.0205(6)
_cell_measurement_reflns_used    13198
_cell_measurement_temperature    293.00(10)
_cell_measurement_theta_max      24.6920
_cell_measurement_theta_min      3.0500
_cell_volume                     6197.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.2634
_diffrn_detector_type            Onyx
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.891
_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    -62.00  31.00   1.00   90.00    --    9.08 -57.00 -60.00   93
  2  \w    -19.00   7.00   1.00   90.00    --    9.08 -57.00 150.00   26
  3  \w    -17.00  76.00   1.00   90.00    --    9.08  57.00  90.00   93
  4  \w     32.00  98.00   1.00   90.00    --    9.08-178.00 150.00   66
  5  \w    -83.00  11.00   1.00   90.00    --  -10.64 -57.00-150.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Onyx'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0122848000
_diffrn_orient_matrix_UB_12      0.0045392000
_diffrn_orient_matrix_UB_13      -0.0361824000
_diffrn_orient_matrix_UB_21      0.0345264000
_diffrn_orient_matrix_UB_22      0.0232784000
_diffrn_orient_matrix_UB_23      0.0043846000
_diffrn_orient_matrix_UB_31      0.0376020000
_diffrn_orient_matrix_UB_32      -0.0198884000
_diffrn_orient_matrix_UB_33      -0.0031397000
_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  0.0862
_diffrn_reflns_av_unetI/netI     0.1021
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            68248
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.266
_diffrn_reflns_theta_min         2.752
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.240
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.945
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       block
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.129
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         15063
_refine_ls_number_restraints     152
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1269
_refine_ls_R_factor_gt           0.0653
_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^)+(0.0663P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8109
_reflns_number_total             15063
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04890a2.cif
_cod_data_source_block           28af2
_cod_depositor_comments          'Adding full bibliography for 7060152.cif.'
_cod_database_code               7060152
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C92 H120 Al4 N4 O32 S8'
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.923
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O13-H13
 0.95 with sigma of 0.01
 O14-H14
 0.95 with sigma of 0.01
 C30A-C27 \\sim C30B-C27 \\sim C28A-C27 \\sim C28B-C27 \\sim C29A-C27 \\sim
C29B-C27
 with sigma of 0.01
 C19B-C17 \\sim C19A-C17 \\sim C18B-C17 \\sim C18A-C17 \\sim C20B-C17 \\sim
C20A-C17
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C27 \\sim C28A \\sim C28B \\sim C29A \\sim C29B \\sim C30A \\sim C30B: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C18A \\sim C18B \\sim C19A \\sim C19B \\sim C20A \\sim C20B: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C37 \\sim C38 \\sim C38 \\sim C39 \\sim C40: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 1.7A
Uanis(C38) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29B)=Sof(H29D)=Sof(H29E)=
 Sof(H29F)=Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29A)=Sof(H29A)=Sof(H29B)=
 Sof(H29C)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
 Sof(C18B)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19B)=Sof(H19D)=Sof(H19E)=
 Sof(H19F)=Sof(C20B)=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(2)
 Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19A)=Sof(H19A)=Sof(H19B)=
 Sof(H19C)=Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C13(H13A), C15(H15), C24(H24), C26(H26), C33(H33), C35(H35),
 C41(H41), C44(H44)
5.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C18A(H18A,H18B,H18C),
 C18B(H18D,H18E,H18F), C19A(H19A,H19B,H19C), C19B(H19D,H19E,H19F), C20A(H20A,
 H20B,H20C), C20B(H20D,H20E,H20F), C28A(H28A,H28B,H28C), C28B(H28D,H28E,H28F),
 C29A(H29A,H29B,H29C), C29B(H29D,H29E,H29F), C30A(H30A,H30B,H30C), C30B(H30D,
 H30E,H30F), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C),
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              13849
_shelx_fab_checksum              24982
_olex2_date_sample_data_collection 2014-01-30
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop in perfluoroether oil'
_olex2_submission_original_sample_id 28AF2
_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 1.214
_oxdiff_exptl_absorpt_empirical_full_min 0.825