An air-stable anionic two-dimensional semiconducting metal-thiolate network and its exfoliation into ultrathin few-layer nanosheets.
Zeng, Qi; Wang, Lei; Huang, Yitao; Zheng, Sai-Li; He, Yonghe; He, Jun; Liao, Wei-Ming; Xu, Gang; Zeller, Matthias; Xu, Zhengtao; Chemical communications (Cambridge, England) 56 (2020) 3645–3648; doi:10.1039/c9cc09349d

data_7126034
_publ_section_title
;
 An air-stable anionic two-dimensional semiconducting metal-thiolate
 network and its exfoliation into ultrathin few-layer nanosheets.
;
_journal_issue                   25
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3645
_journal_page_last               3648
_journal_paper_doi               10.1039/c9cc09349d
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety
'C16 Eu F4 O8 S4, H16 N4, 0.25(C8 H32 N4), H2 O'
_chemical_formula_sum            'C18 H26 Eu F4 N5 O9 S4'
_chemical_formula_weight         812.64
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-07-09
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.05.30 svn.r3610 for OlexSys, GUI svn.r5794)
;
_audit_update_record
;
2019-07-19 deposited with the CCDC.	2020-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.7820(3)
_cell_length_b                   12.782
_cell_length_c                   8.4363(2)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    230.0
_cell_measurement_theta_max      41.96
_cell_measurement_theta_min      2.89
_cell_volume                     1378.32(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      230.0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            26569
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.311
_diffrn_reflns_theta_min         3.188
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.662
_exptl_absorpt_correction_T_max  0.852
_exptl_absorpt_correction_T_min  0.760
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'solvothermal method'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.456
_refine_diff_density_min         -1.375
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         3342
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0214
_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^)+(0.0197P)^2^+1.0864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0466
_refine_ls_wR_factor_ref         0.0510
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3028
_reflns_number_total             3342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09349d2.cif
_cod_data_source_block           Eu_dfdmt
_cod_depositor_comments          'Adding full bibliography for 7126034.cif.'
_cod_original_cell_volume        1378.32(7)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7126034
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.857
_shelx_estimated_absorpt_t_min   0.675
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O3-H3
 0.84 with sigma of 0.02
 H3-H3_$1
 1.36 with sigma of 0.02
 N1-C6 \\sim N1-C5
 with sigma of 0.02
 N2-H2A \\sim N2-H2B \\sim N2-H2C \\sim N2-H2D
 with sigma of 0.02
 H2A-H2B \\sim H2A-H2C \\sim H2A-H2D \\sim H2B-H2C \\sim H2B-H2D \\sim H2C-H2D
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N1 \\sim C6 \\sim C5: within 2.6A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2.6A
4. Others
 Fixed Sof: N1(0.25) H1A(0.25) H1B(0.25) C6(0.25) H6A(0.25) H6B(0.25)
 H6C(0.25) C5(0.25) H5A(0.25) H5B(0.25) H5C(0.25) H3(0.5)
5.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
5.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C5(H5A,H5B,H5C)
;
_olex2_submission_special_instructions 'No special instructions were received'