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_7714557
_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 H10 Co0.5 O4 P S2'
_chemical_formula_sum            'C12 H10 Co0.5 O4 P S2'
_chemical_formula_weight         342.75
_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                 93.8460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.1542(2)
_cell_length_b                   7.93590(10)
_cell_length_c                   15.1100(2)
_cell_measurement_reflns_used    13171
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.6090
_cell_measurement_theta_min      3.9900
_cell_volume                     2650.56(5)
_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 0.999
_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     31.00  57.00   0.50    0.50    --   43.75  57.00 -30.00   52
  2  \w     21.00 108.00   0.50    0.50    --   43.75  77.00-120.00  174
  3  \w    137.00 162.00   0.50    2.00    --  110.00 108.00-112.00   50
  4  \w    121.00 146.00   0.50    2.00    --  110.00 125.00-180.00   50
  5  \w     90.00 158.00   0.50    2.00    --  110.00  61.00 -90.00  136
  6  \w    128.00 153.00   0.50    2.00    --  110.00  45.00 -90.00   50
  7  \w    126.00 151.00   0.50    2.00    --  110.00  15.00 -90.00   50
  8  \w     98.00 148.00   0.50    2.00    --  110.00  61.00 -60.00  100
  9  \w    123.00 149.00   0.50    2.00    --  110.00  45.00  30.00   52
 10  \w    116.00 164.00   0.50    2.00    --  110.00  30.00  90.00   96
 11  \w     98.00 138.00   0.50    2.00    --  110.00  45.00 -30.00   80
 12  \w     83.00 117.00   0.50    2.00    --  110.00  15.00 -90.00   68
 13  \w    100.00 126.00   0.50    2.00    --  110.00  30.00-150.00   52
 14  \w     60.00 123.00   0.50    2.00    --  110.00 -45.00 -60.00  126
 15  \w    101.00 137.00   0.50    2.00    --  110.00 -77.00 -90.00   72
 16  \w    106.00 132.00   0.50    2.00    --  110.00 -88.00 -17.29   52
 17  \w     79.00 105.00   0.50    2.00    --  110.00-125.00 -30.00   52
 18  \w     87.00 113.00   0.50    2.00    --  110.00 -61.00 -90.00   52
 19  \w     75.00 101.00   0.50    2.00    --  110.00 -77.00-150.00   52
 20  \w     58.00 112.00   0.50    2.00    --  110.00-125.00-150.00  108
 21  \w     63.00  99.00   0.50    2.00    --  110.00 -94.00-120.00   72
 22  \w     45.00  71.00   0.50    2.00    --  110.00 -61.00 -90.00   52
 23  \w     60.00 105.00   0.50    2.00    --  110.00 -94.00 -30.00   90
 24  \w     86.00 111.00   0.50    2.00    --  110.00 -77.00  60.00   50
 25  \w     63.00 103.00   0.50    2.00    --  110.00-108.00 151.00   80
 26  \w     92.00 117.00   0.50    2.00    --  110.00 -77.00 150.00   50
 27  \w     88.00 114.00   0.50    2.00    --  110.00 -45.00 150.00   52
 28  \w     60.00  86.00   0.50    2.00    --  110.00-125.00 150.00   52
 29  \w     68.00 106.00   0.50    2.00    --  110.00 -94.00 150.00   76
 30  \w     51.00  77.00   0.50    2.00    --  110.00 -77.00 150.00   52
 31  \w     40.00  65.00   0.50    2.00    --  110.00 -45.00 150.00   50
 32  \w     42.00 112.00   0.50    2.00    --  110.00-125.00 120.00  140
 33  \w     48.00 126.00   0.50    2.00    --  110.00 -30.00  30.00  156
 34  \w     81.00 138.00   0.50    2.00    --  110.00  77.00  90.00  114
 35  \w     88.00 167.00   0.50    2.00    --  110.00  77.00  30.00  158
 36  \w     52.00  92.00   0.50    2.00    --  110.00 -77.00 -90.00   80
 37  \w     41.00  79.00   0.50    2.00    --  110.00 -88.00 -17.29   76
 38  \w     51.00  76.00   0.50    2.00    --  110.00 -94.00  30.00   50
 39  \w     22.00  81.00   0.50    0.50    --   43.75-108.00 151.00  118
 40  \w    -13.00  35.00   0.50    0.50    --   -0.75 -94.00  90.00   96
 41  \w     19.00 106.00   0.50    0.50    --   43.75  19.00 120.00  174
 42  \w     39.00  72.00   0.50    2.00    --  110.00 -94.00-150.00   66
 43  \w    -27.00  44.00   0.50    0.50    --   43.75 -38.00-180.00  142
 44  \w    -45.00 -20.00   0.50    0.50    --   -0.75 108.00-112.00   50
;
_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      0.0257374000
_diffrn_orient_matrix_UB_12      0.1781939000
_diffrn_orient_matrix_UB_13      -0.0122985000
_diffrn_orient_matrix_UB_21      -0.0634219000
_diffrn_orient_matrix_UB_22      0.0631737000
_diffrn_orient_matrix_UB_23      -0.0324615000
_diffrn_orient_matrix_UB_31      -0.0131527000
_diffrn_orient_matrix_UB_32      0.0441539000
_diffrn_orient_matrix_UB_33      0.0960944000
_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  0.0383
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28423
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.893
_diffrn_reflns_theta_min         4.000
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.604
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45476
_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            pink
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_description       colorless
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.024
_refine_diff_density_max         1.566
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5522
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0713
_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^)+(0.0236P)^2^+47.8444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2195
_refine_ls_wR_factor_ref         0.2198
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5363
_reflns_number_total             5522
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03153e2.cif
_cod_data_source_block           gl656_2
_cod_original_formula_sum        'C12 H10 Co0.50 O4 P S2'
_cod_database_code               7714557
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co P S2 C12 O3 H7'
_diffrn_oxdiff_ac4_digest_frames
;
01a4ea9daf1bab761e849d0e86408f2c3b03620da75
;
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Uiso: H7A(0.001)
3.a Free rotating group:
 O8(H8A,H8B), O7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C14(H14), C6(H6), C18(H18), C5(H5), C17(H17), C11(H11), C8(H8),
 C23(H23), C20(H20), C22(H22), C9(H9), C10(H10), C21(H21)
3.c Idealised tetrahedral OH refined as rotating group:
 O4(H4), O1(H1)
;
_shelx_res_checksum              93757
_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 1.719
_oxdiff_exptl_absorpt_empirical_full_min 0.706