Supramolecular Aggregation in Dithia-arsoles: Chlorides, Cations and N-centered Paddlewheels
Tran, Thao Thi-Phuong; Ould, Darren; Wilkins, Lewis; Wright, Dominic S.; Melen, Rebecca; Rawson, Jeremy Michael; CrystEngComm  (2017) –; doi:10.1039/C7CE01117B

data_7228718
_publ_section_title
;
 Supramolecular Aggregation in Dithia-arsoles: Chlorides, Cations and
 N-centered Paddlewheels
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01117B
_journal_year                    2017
_chemical_formula_moiety         'C7 H6 As S2, Al Cl 4'
_chemical_formula_sum            'C7 H6 Al As Cl4 S2'
_chemical_formula_weight         397.94
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-28 deposited with the CCDC.
2017-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.135(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4720(7)
_cell_length_b                   7.0562(5)
_cell_length_c                   17.819(2)
_cell_measurement_reflns_used    15704
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      22.46
_cell_measurement_theta_min      1.02
_cell_volume                     1410.2(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick 2014)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1501
_diffrn_reflns_av_unetI/netI     0.0973
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7859
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        22.389
_diffrn_reflns_theta_max         22.389
_diffrn_reflns_theta_min         3.575
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.492
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (blessing 1995)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.874
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         2.393
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         1959
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.0879
_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^)+(0.0739P)^2^+21.9094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2281
_refine_ls_wR_factor_ref         0.2366
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1528
_reflns_number_total             1959
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01117b2.cif
_cod_data_source_block           dw1041
_cod_database_code               7228718
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.641
_shelx_estimated_absorpt_t_max   0.966
_exptl_absorpt_special_details
; 
 Tiny crystal; very poor data; common, isotropic displacement parameters
 for the carbon atoms; the methyl hydrogen atoms were constrained to 
obey the space group symmetry. Isomorphous with the GaCl4 salt which
diffracted and refined better.
;
_shelx_res_checksum              43057