A series of oxysulfides RE<sub>2</sub>M<sub>2</sub>S<sub>3</sub>O<sub>4</sub> (RE = Y, Tm; M = Zr, Hf) featuring a unique MS<sub>3</sub>O<sub>4</sub> motif and {[M<sub>2</sub>S<sub>3</sub>O<sub>4</sub>]<sup>8-</sup>}<sub>∞ </sub> wrinkle layer.
Lu, Zhen-Tao; Yang, Si-Han; Liu, Wenlong; Guo, Sheng-Ping; Chemical communications (Cambridge, England) 57 (2021) 3500–3503; doi:10.1039/d1cc00351h

data_7128000
_publ_section_title
;
 A series of oxysulfides
 RE<sub>2</sub>M<sub>2</sub>S<sub>3</sub>O<sub>4</sub> (RE = Y, Tm; M =
 Zr, Hf) featuring a unique MS<sub>3</sub>O<sub>4</sub> motif and
 {[M<sub>2</sub>S<sub>3</sub>O<sub>4</sub>]<sup>8-</sup>}<sub>\\infty
 </sub> wrinkle layer.
;
_journal_issue                   28
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3500
_journal_page_last               3503
_journal_paper_doi               10.1039/d1cc00351h
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C24 H19 N9 O5 Pt'
_chemical_formula_sum            'C24 H19 N9 O5 Pt'
_chemical_formula_weight         708.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2021-01-05 deposited with the CCDC.	2021-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                92.7868(16)
_cell_angle_beta                 90.0429(14)
_cell_angle_gamma                106.8637(16)
_cell_formula_units_Z            2
_cell_length_a                   7.40510(12)
_cell_length_b                   8.24493(17)
_cell_length_c                   21.2074(4)
_cell_measurement_reflns_used    33661
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.6740
_cell_measurement_theta_min      2.7040
_cell_volume                     1237.51(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1417
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.940
_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    -25.00  52.00   1.00    3.00    --   11.41 -99.00  30.00   77
  2  \w    -13.00  86.00   1.00    3.00    --   11.41  38.00 -60.00   99
  3  \w    -17.00  85.00   1.00    3.00    --   11.41  57.00-180.00  102
  4  \w    -21.00  88.00   1.00    3.00    --   11.41  77.00  30.00  109
  5  \w    -25.00  52.00   1.00    3.00    --   11.41 -99.00 120.00   77
  6  \w    -45.00  64.00   1.00    3.00    --  -12.35  77.00 150.00  109
  7  \w    -41.00  61.00   1.00    3.00    --  -12.35  57.00 -90.00  102
  8  \w    -88.00 -37.00   1.00    3.00    --  -12.35 154.00 -85.13   51
  9  \w    -63.00  36.00   1.00    3.00    --   11.41 -38.00  30.00   99
 10  \w    -71.00 -22.00   1.00    3.00    --  -12.35 129.00  68.19   49
 11  \w    -83.00 -32.00   1.00    3.00    --  -12.35 147.00   0.35   51
 12  \w    -81.00 -31.00   1.00    3.00    --  -12.35 145.00-127.49   50
 13  \w    -84.00 -33.00   1.00    3.00    --  -12.35 149.00  92.45   51
 14  \w    -67.00 -16.00   1.00    3.00    --  -12.35 122.00 162.00   51
 15  \w    -77.00  -8.00   1.00    3.00    --   11.41   0.00-120.00   69
 16  \w    -77.00 100.00   1.00    3.00    --   11.41   0.00-180.00  177
 17  \w    -77.00 100.00   1.00    3.00    --   11.41   0.00-150.00  177
 18  \w    -25.00  29.00   1.00    3.00    --  -12.35 -99.00-120.00   54
 19  \w    -67.00 -16.00   1.00    3.00    --  -12.35 122.00-152.38   51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0223181000
_diffrn_orient_matrix_UB_12      -0.0789945000
_diffrn_orient_matrix_UB_13      -0.0174938000
_diffrn_orient_matrix_UB_21      -0.0231218000
_diffrn_orient_matrix_UB_22      -0.0431235000
_diffrn_orient_matrix_UB_23      0.0283611000
_diffrn_orient_matrix_UB_31      -0.0948026000
_diffrn_orient_matrix_UB_32      0.0015067000
_diffrn_orient_matrix_UB_33      -0.0033485000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            59521
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.027
_diffrn_reflns_theta_min         2.585
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.725
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.203
_refine_diff_density_min         -1.130
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         6820
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0223
_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^)+(0.0172P)^2^+0.8966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0424
_refine_ls_wR_factor_ref         0.0439
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6317
_reflns_number_total             6820
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00351h2.cif
_cod_data_source_block           hs33
_cod_depositor_comments
'Adding full bibliography for 7127998--7128000.cif.'
_cod_database_code               7128000
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H20 N2 O2 Pt'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.01
_olex2_refinement_description
;
The naphthalimide ring was modeled as disordered over two positions related by a small twist about 
the N22-C21 bond. The occupancy was linked to a free variable which refined to 48:52. 
Some SIMU restraints were used to give some of the disordered atoms similar thermal parameters 
to neighbouring atoms. The hydrogen on the OH was located in a difference map but placed at a 
calculated position for the refinement. 

1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
C21 \\sim N22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim
C29 \\sim C30: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C20 \\sim C21A \\sim N22A \\sim C34A \\sim C32A \\sim C31A: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
3. Others
 Sof(C23A)=Sof(O23A)=Sof(C24A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=
 Sof(C27A)=Sof(H27A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=Sof(C31A)=
 Sof(H31A)=Sof(C32A)=Sof(C34A)=Sof(O34A)=Sof(N22A)=Sof(C21A)=Sof(H21C)=
 Sof(H21D)=1-FVAR(1)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(N22)=Sof(C23)=Sof(O23)=Sof(C24)=Sof(C25)=
 Sof(H25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=Sof(C29)=Sof(H29)=Sof(C30)=
 Sof(H30)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(C34)=Sof(O34)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C21A(H21C,H21D)
4.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C25(H25), C25A(H25A), C26(H26), C26A(H26A), C27(H27),
 C27A(H27A), C29(H29), C29A(H29A), C30(H30), C30A(H30A), C31(H31), C31A(H31A)
4.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              98130
_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 1.918
_oxdiff_exptl_absorpt_empirical_full_min 0.709