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_7714555
_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 O3 P S2'
_chemical_formula_sum            'C12 H9 O3 P S2'
_chemical_formula_weight         296.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-10
_audit_creation_method
;
Olex2 1.2-ac4
(compiled 2018.05.17 svn.r3504 for Rigaku Oxford Diffraction, GUI svn.r5492)
;
_audit_update_record
;
2023-09-21 deposited with the CCDC.	2023-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.80963(5)
_cell_length_b                   10.61773(11)
_cell_length_c                   24.0170(2)
_cell_measurement_reflns_used    14093
_cell_measurement_temperature    292.85(10)
_cell_measurement_theta_max      75.5300
_cell_measurement_theta_min      3.6500
_cell_volume                     1226.48(2)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.85(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Eiger 1M'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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     29.00 117.00   0.50    0.50    --   43.75  38.00 -30.00  176
  2  \w    100.00 171.00   0.50    2.00    --  110.00  85.00  -4.00  142
  3  \w     97.00 171.00   0.50    2.00    --  110.00  45.00 150.00  148
  4  \w     97.00 171.00   0.50    2.00    --  110.00  45.00  60.00  148
  5  \w     97.00 171.00   0.50    2.00    --  110.00  45.00 120.00  148
  6  \w     90.00 161.00   0.50    2.00    --  110.00  30.00  30.00  142
  7  \w     89.00 171.00   0.50    2.00    --  110.00  61.00 -60.00  164
  8  \w     97.00 171.00   0.50    2.00    --  110.00  45.00-180.00  148
  9  \w     90.00 171.00   0.50    2.00    --  110.00  30.00 -60.00  162
 10  \w     90.00 171.00   0.50    2.00    --  110.00  30.00   0.00  162
 11  \w     90.00 171.00   0.50    2.00    --  110.00  30.00-120.00  162
 12  \w     76.00 171.00   0.50    2.00    --  110.00  15.00 120.00  190
 13  \w     43.00 142.00   0.50    2.00    --  110.00 -85.00-123.00  198
 14  \w     34.00 129.00   0.50    2.00    --  110.00 -30.00 -60.00  190
 15  \w     46.00 139.00   0.50    2.00    --  110.00 -77.00-150.00  186
 16  \w     44.00 130.00   0.50    2.00    --  110.00 -61.00   0.00  172
 17  \w     38.00 106.00   0.50    2.00    --  110.00 -94.00  30.00  136
 18  \w     39.00 112.00   0.50    2.00    --  110.00-125.00 -30.00  146
 19  \w     38.00 123.00   0.50    2.00    --  110.00 -45.00  90.00  170
 20  \w     34.00 129.00   0.50    2.00    --  110.00 -30.00 150.00  190
 21  \w     39.00 112.00   0.50    2.00    --  110.00-125.00  60.00  146
 22  \w     38.00 106.00   0.50    2.00    --  110.00 -94.00-150.00  136
 23  \w     26.00 111.00   0.50    0.50    --   43.75  57.00-150.00  170
 24  \w     15.00 108.00   0.50    0.50    --   43.75  77.00  30.00  186
 25  \w     26.00 111.00   0.50    0.50    --   43.75  57.00  90.00  170
 26  \w     15.00 108.00   0.50    0.50    --   43.75  77.00   0.00  186
 27  \w     15.00 108.00   0.50    0.50    --   43.75  77.00 150.00  186
 28  \w     15.00 108.00   0.50    0.50    --   43.75  77.00  60.00  186
 29  \w     15.00 108.00   0.50    0.50    --   43.75  77.00 -90.00  186
 30  \w     15.00 108.00   0.50    0.50    --   43.75  77.00-150.00  186
 31  \w     15.00 108.00   0.50    0.50    --   43.75  77.00 -60.00  186
 32  \w     15.00 108.00   0.50    0.50    --   43.75  77.00 120.00  186
 33  \w    -21.00  31.00   0.50    0.50    --   -0.75 -85.00-123.00  104
 34  \w    -13.00  36.00   0.50    0.50    --   -0.75 -94.00-180.00   98
 35  \w    -21.00  76.00   0.50    0.50    --   43.75 -85.00-123.00  194
 36  \w     -2.00  83.00   0.50    0.50    --   43.75 -99.00  30.00  170
 37  \w     -2.00  83.00   0.50    0.50    --   43.75 -99.00  90.00  170
 38  \w    -21.00  72.00   0.50    0.50    --   43.75 -77.00 120.00  186
 39  \w    -33.00  43.00   0.50    0.50    --   -0.75  85.00  -4.00  152
 40  \w    -34.00  68.00   0.50    0.50    --   43.75 -19.00-150.00  204
;
_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      0.1349580000
_diffrn_orient_matrix_UB_12      -0.0567940000
_diffrn_orient_matrix_UB_13      -0.0524685000
_diffrn_orient_matrix_UB_21      -0.0937583000
_diffrn_orient_matrix_UB_22      0.1153528000
_diffrn_orient_matrix_UB_23      -0.0340747000
_diffrn_orient_matrix_UB_31      0.2749518000
_diffrn_orient_matrix_UB_32      0.0672567000
_diffrn_orient_matrix_UB_33      0.0141300000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            23440
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.890
_diffrn_reflns_theta_min         3.681
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.158
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.536
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.23a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       plate
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.184
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 984 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(6)
_refine_ls_extinction_coef       0.0005(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0240
_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^)+(0.0370P)^2^+0.3325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0660
_reflns_Friedel_coverage         0.666
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                2476
_reflns_number_total             2533
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03153e2.cif
_cod_data_source_block           paj719a-1
_cod_database_code               7714555
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C12 H9 O3 P S2 '
_diffrn_oxdiff_ac4_digest_frames
;
01b1b344d8eb41fa769700420691ce998506668a610
;
_reflns_odcompleteness_completeness 99.93
_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.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C12(H12), C11(H11), C7(H7), C4(H4), C6(H6), C5(H5)
2.b Idealised tetrahedral OH refined as rotating group:
 O16(H16), O18(H18)
;
_shelx_res_checksum              77901
_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 1.313
_oxdiff_exptl_absorpt_empirical_full_min 0.833