A new series of magnetic and luminescent layered hybrid materials obtained from thianthrene phosphonic acid: M(H<sub>2</sub>O)PO<sub>3</sub>-S<sub>2</sub>C<sub>12</sub>H<sub>7</sub> (M = Cu, Zn) and M(H<sub>2</sub>O)<sub>2</sub>(PO<sub>2</sub>OH-S<sub>2</sub>C<sub>12</sub>H<sub>7</sub>)<sub>2</sub> (M = Mn, Co).
Letheux, Geoffrey; Ganesan, Parameshwari; Veillon, Fabien; Varignon, Julien; Perez, Olivier; Cardin, Julien; Labbé, Christophe; Rogez, Guillaume; Ligeour, Mathilde; Jaffrès, Paul-Alain; Rueff, Jean-Michel; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt03153e

data_7714556
_publ_section_title
;
 A new series of magnetic and luminescent layered hybrid materials
 obtained from thianthrene phosphonic acid:
 M(H<sub>2</sub>O)PO<sub>3</sub>-S<sub>2</sub>C<sub>12</sub>H<sub>7</sub>
 (M = Cu, Zn) and
 M(H<sub>2</sub>O)<sub>2</sub>(PO<sub>2</sub>OH-S<sub>2</sub>C<sub>12</sub>H<sub>7</sub>)<sub>2</sub>
 (M = Mn, Co).
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt03153e
_journal_year                    2023
_chemical_formula_moiety         'C12 H9 O4 P S2 Zn'
_chemical_formula_sum            'C12 H9 O4 P S2 Zn'
_chemical_formula_weight         377.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2023-09-21 deposited with the CCDC.	2023-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.283(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.0947(5)
_cell_length_b                   7.8428(2)
_cell_length_c                   7.8758(2)
_cell_measurement_reflns_used    4892
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.2570
_cell_measurement_theta_min      4.0400
_cell_volume                     1358.96(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Eiger 1M'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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    -17.00  68.00   0.50    8.24    --   -0.75  53.00 -24.00  170
  2  \w     28.00 113.00   0.50    8.24    --   43.75  53.00 -24.00  170
  3  \w     94.00 171.00   0.50    8.24    --  110.00  53.00 -24.00  154
  4  \w    133.00 171.00   0.50    8.24    --  110.00  61.00   0.00   76
  5  \w    146.00 171.00   0.50    8.24    --  110.00  75.00  73.61   50
  6  \w    123.00 148.00   0.50    8.24    --  110.00 125.00  60.00   50
  7  \w    117.00 171.00   0.50    8.24    --  110.00  69.00  94.11  108
  8  \w    125.00 154.00   0.50    8.24    --  110.00  45.00 120.00   58
  9  \w    116.00 141.00   0.50    8.24    --  110.00  15.00  90.00   50
 10  \w    103.00 129.00   0.50    8.24    --  110.00  61.00  30.00   52
 11  \w    108.00 171.00   0.50    8.24    --  110.00  30.00 -30.00  126
 12  \w    125.00 152.00   0.50    8.24    --  110.00  64.00-130.26   54
 13  \w    137.00 171.00   0.50    8.24    --  110.00  61.00-150.00   68
 14  \w    121.00 147.00   0.50    8.24    --  110.00 125.00-150.00   52
 15  \w    118.00 155.00   0.50    8.24    --  110.00 125.00-120.00   74
 16  \w    117.00 171.00   0.50    8.24    --  110.00 125.00 -60.00  108
 17  \w     90.00 171.00   0.50    8.24    --  110.00  30.00  30.00  162
 18  \w     92.00 171.00   0.50    8.24    --  110.00  32.00 -55.36  158
 19  \w     89.00 171.00   0.50    8.24    --  110.00  61.00 -90.00  164
 20  \w     89.00 171.00   0.50    8.24    --  110.00  61.00-120.00  164
 21  \w     91.00 117.00   0.50    8.24    --  110.00 -45.00 -30.00   52
 22  \w     77.00 127.00   0.50    8.24    --  110.00  15.00  60.00  100
 23  \w     97.00 123.00   0.50    8.24    --  110.00  45.00  30.00   52
 24  \w     99.00 125.00   0.50    8.24    --  110.00  45.00  90.00   52
 25  \w     81.00 171.00   0.50    8.24    --  110.00  77.00  60.00  180
 26  \w     89.00 171.00   0.50    8.24    --  110.00  61.00  60.00  164
 27  \w     91.00 134.00   0.50    8.24    --  110.00  59.00  95.51   86
 28  \w     81.00 171.00   0.50    8.24    --  110.00  77.00  30.00  180
 29  \w     92.00 117.00   0.50    8.24    --  110.00  61.00 -60.00   50
 30  \w     83.00 171.00   0.50    8.24    --  110.00  73.00  21.93  176
 31  \w     89.00 152.00   0.50    8.24    --  110.00  61.00 120.00  126
 32  \w     82.00 116.00   0.50    8.24    --  110.00  75.00  73.61   68
 33  \w     85.00 114.00   0.50    8.24    --  110.00  69.00  94.11   58
 34  \w     83.00 115.00   0.50    8.24    --  110.00  77.00 109.76   64
 35  \w     86.00 112.00   0.50    8.24    --  110.00  77.00 120.00   52
 36  \w     81.00 171.00   0.50    8.24    --  110.00  77.00  90.00  180
 37  \w     76.00 171.00   0.50    8.24    --  110.00  15.00 120.00  190
 38  \w     80.00 171.00   0.50    8.24    --  110.00  80.00  34.62  182
 39  \w     67.00 109.00   0.50    8.24    --  110.00   0.00 120.00   84
 40  \w     44.00 107.00   0.50    8.24    --  110.00 -61.00 150.00  126
 41  \w     38.00  83.00   0.50    8.24    --  110.00 -94.00 120.00   90
 42  \w     34.00 129.00   0.50    8.24    --  110.00 -30.00  60.00  190
 43  \w     80.00 105.00   0.50    8.24    --  110.00-125.00 -60.00   50
 44  \w     61.00  87.00   0.50    8.24    --  110.00-125.00  30.00   52
 45  \w     43.00  90.00   0.50    8.24    --  110.00-135.00 -33.04   94
 46  \w     41.00 126.00   0.50    8.24    --  110.00 -53.00-168.00  170
 47  \w     46.00  75.00   0.50    8.24    --  110.00 -45.00 -30.00   58
 48  \w     38.00 123.00   0.50    8.24    --  110.00 -45.00-150.00  170
 49  \w     39.00 106.00   0.50    8.24    --  110.00-125.00-180.00  134
 50  \w     -2.00  83.00   0.50    8.24    --   43.75 -99.00 -30.00  170
 51  \w     -2.00  83.00   0.50    8.24    --   43.75 -99.00-180.00  170
 52  \w    -25.00  60.00   0.50    8.24    --   43.75 -53.00-168.00  170
 53  \w     26.00 111.00   0.50    8.24    --   43.75  57.00   0.00  170
 54  \w     26.00 111.00   0.50    8.24    --   43.75  57.00  60.00  170
 55  \w     26.00 111.00   0.50    8.24    --   43.75  57.00 120.00  170
 56  \w     -2.00  83.00   0.50    8.24    --   43.75 -99.00  30.00  170
 57  \w    -70.00  15.00   0.50    8.24    --   -0.75 -53.00-168.00  170
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Eiger 1M'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1719963000
_diffrn_orient_matrix_UB_12      -0.0155587000
_diffrn_orient_matrix_UB_13      -0.0275774000
_diffrn_orient_matrix_UB_21      0.0636526000
_diffrn_orient_matrix_UB_22      -0.1246543000
_diffrn_orient_matrix_UB_23      0.0510166000
_diffrn_orient_matrix_UB_31      -0.0703985000
_diffrn_orient_matrix_UB_32      -0.1509699000
_diffrn_orient_matrix_UB_33      -0.0392624000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0797
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            27137
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.944
_diffrn_reflns_theta_min         4.019
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.596
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.23a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_description       needle
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.073
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.018
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0372
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1283
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2449
_reflns_number_total             2810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03153e2.cif
_cod_data_source_block           gl313_1
_cod_database_code               7714556
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'S P O3 C12 H7'
_diffrn_oxdiff_ac4_digest_frames
;
0102a4255d4e1154baa232b77341b5b7a6000259dfa
;
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     50.38
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Free rotating group:
 O4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C8(H8), C11(H11), C10(H10), C9(H9)
;
_shelx_res_checksum              48800
_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 1.445
_oxdiff_exptl_absorpt_empirical_full_min 0.742