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_7714558
_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 Cu O4 P S2'
_chemical_formula_sum            'C12 H9 Cu O4 P S2'
_chemical_formula_weight         375.82
_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             2023-09-05
_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                 95.297(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.0156(5)
_cell_length_b                   7.6616(2)
_cell_length_c                   7.5811(2)
_cell_measurement_reflns_used    5079
_cell_measurement_temperature    290.15(10)
_cell_measurement_theta_max      73.5490
_cell_measurement_theta_min      4.0550
_cell_volume                     1273.28(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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_area_resol_mean 13.3333
_diffrn_detector_type            'Eiger 1M'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_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    -76.00  17.00   0.50    0.20    --   -0.75 -33.00 149.00  186
  2  \w     26.00 119.00   0.50    0.20    --   43.75  33.00 -51.00  186
  3  \w    -31.00  61.00   0.50    0.20    --   43.75 -33.00 149.00  184
  4  \w     92.00 171.00   0.50    0.40    --  110.00  33.00 -51.00  158
  5  \w     35.00 128.00   0.50    0.40    --  110.00 -33.00 149.00  186
  6  \w    -18.00  74.00   0.50    0.20    --   -0.75  33.00 -51.00  184
  7  \w     26.00 111.00   0.50    0.20    --   43.75  57.00-120.00  170
  8  \w     -2.00  83.00   0.50    0.20    --   43.75 -99.00  90.00  170
  9  \w     26.00 111.00   0.50    0.20    --   43.75  57.00   0.00  170
 10  \w    -21.00  72.00   0.50    0.20    --   43.75 -77.00 150.00  186
 11  \w     15.00 108.00   0.50    0.20    --   43.75  77.00  30.00  186
 12  \w     26.00 111.00   0.50    0.20    --   43.75  57.00  30.00  170
 13  \w     85.00 171.00   0.50    0.40    --  110.00  69.00 -28.77  172
 14  \w     89.00 171.00   0.50    0.40    --  110.00  61.00  60.00  164
 15  \w     80.00 171.00   0.50    0.40    --  110.00  80.00   1.85  182
 16  \w     94.00 171.00   0.50    0.40    --  110.00 125.00-180.00  154
 17  \w     76.00 171.00   0.50    0.40    --  110.00  15.00  60.00  190
 18  \w     44.00 130.00   0.50    0.40    --  110.00 -61.00  30.00  172
 19  \w     81.00 171.00   0.50    0.40    --  110.00  77.00  60.00  180
 20  \w     38.00 106.00   0.50    0.40    --  110.00 -94.00-180.00  136
 21  \w     39.00 112.00   0.50    0.40    --  110.00-125.00 120.00  146
 22  \w     89.00 118.00   0.50    0.40    --  110.00  61.00   0.00   58
 23  \w    135.00 169.00   0.50    0.40    --  110.00  61.00   0.00   68
 24  \w     68.00  94.00   0.50    0.40    --  110.00 -61.00-180.00   52
 25  \w     46.00 104.00   0.50    0.40    --  110.00 -45.00 -90.00  116
 26  \w     81.00 107.00   0.50    0.40    --  110.00  77.00   0.00   52
 27  \w     83.00 124.00   0.50    0.40    --  110.00  77.00 -30.00   82
 28  \w    140.00 165.00   0.50    0.40    --  110.00  61.00 120.00   50
 29  \w     69.00 107.00   0.50    0.40    --  110.00-125.00-150.00   76
 30  \w     90.00 117.00   0.50    0.40    --  110.00  61.00  30.00   54
 31  \w     47.00  80.00   0.50    0.40    --  110.00 -45.00  90.00   66
 32  \w     32.00  69.00   0.50    0.40    --  110.00 -15.00  90.00   74
 33  \w     81.00 131.00   0.50    0.40    --  110.00  77.00  90.00  100
 34  \w     98.00 140.00   0.50    0.40    --  110.00 -84.00  35.17   84
 35  \w     59.00  86.00   0.50    0.40    --  110.00 -84.00  35.17   54
 36  \w    116.00 141.00   0.50    0.40    --  110.00 -15.00  90.00   50
 37  \w     81.00 108.00   0.50    0.40    --  110.00  77.00  30.00   54
 38  \w    116.00 171.00   0.50    0.40    --  110.00  77.00 -60.00  110
 39  \w     88.00 113.00   0.50    0.40    --  110.00  67.00  35.46   50
 40  \w    124.00 158.00   0.50    0.40    --  110.00  67.00  35.46   68
 41  \w     42.00  89.00   0.50    0.40    --  110.00-125.00   0.00   94
 42  \w     91.00 132.00   0.50    0.40    --  110.00  30.00  90.00   82
 43  \w     34.00 110.00   0.50    0.40    --  110.00 -30.00  30.00  152
 44  \w     41.00 106.00   0.50    0.40    --  110.00 -94.00  90.00  130
 45  \w    122.00 171.00   0.50    0.40    --  110.00 125.00 -30.00   98
 46  \w     92.00 140.00   0.50    0.40    --  110.00  31.00  43.11   96
 47  \w    116.00 166.00   0.50    0.40    --  110.00  30.00   0.00  100
 48  \w    102.00 128.00   0.50    0.40    --  110.00  61.00 -30.00   52
 49  \w     90.00 115.00   0.50    0.40    --  110.00  61.00 101.76   50
 50  \w     64.00 114.00   0.50    0.40    --  110.00 -61.00-150.00  100
 51  \w     73.00  99.00   0.50    0.40    --  110.00-100.00 132.73   52
 52  \w     98.00 126.00   0.50    0.40    --  110.00  45.00  60.00   56
 53  \w    102.00 128.00   0.50    0.40    --  110.00  45.00  90.00   52
 54  \w     91.00 124.00   0.50    0.40    --  110.00  30.00 120.00   66
 55  \w     90.00 148.00   0.50    0.40    --  110.00  61.00-180.00  116
 56  \w     89.00 135.00   0.50    0.40    --  110.00  61.00 -60.00   92
 57  \w     94.00 120.00   0.50    0.40    --  110.00   0.00 -30.00   52
 58  \w     38.00  64.00   0.50    0.40    --  110.00   0.00 -30.00   52
 59  \w     90.00 116.00   0.50    0.40    --  110.00  61.00  90.00   52
 60  \w     85.00 122.00   0.50    0.40    --  110.00 -45.00  60.00   74
 61  \w     88.00 113.00   0.50    0.40    --  110.00  77.00-120.00   50
 62  \w     69.00  95.00   0.50    0.40    --  110.00 -94.00 -60.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Eiger 1M'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_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            21112
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.140
_diffrn_reflns_theta_min         4.033
_exptl_absorpt_coefficient_mu    6.783
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.961
_exptl_crystal_description       platelets
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.078
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.916
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1022P)^2^+1.4853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2292
_reflns_number_total             2651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03153e2.cif
_cod_data_source_block           gl419_2
_cod_database_code               7714558
_shelx_shelxl_version_number     2018/3
_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:
 C6(H6), C2(H2), C3(H3), C8(H8), C11(H11), C10(H10), C9(H9)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              64859
_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
;