Synthesis, structure, and characterization of a series of Ag(i), Cu(ii) and Ni(ii) complexes based on 2,5-dimethyl-1,3,4-thiodiazole
Liu, Ju Yan; Liu, Zhong Yi; Zhang, Li Jun; Wang, You You; Yang, Pan; Wang, Ying; Ding, Bin; Zhao, Xiao Jun; CrystEngComm 15 (2013) 6413–; doi:10.1039/c3ce40672e

data_7210291
_publ_section_title
;
 Synthesis, structure, and characterization of a series of Ag(i), Cu(ii)
 and Ni(ii) complexes based on 2,5-dimethyl-1,3,4-thiodiazole
;
_journal_issue                   32
_journal_name_full               CrystEngComm
_journal_page_first              6413
_journal_paper_doi               10.1039/c3ce40672e
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C16 H24 Ag2 N8 S3, 4(As0.5 F3)'
_chemical_formula_sum            'C16 H24 Ag2 As2 F12 N8 S3'
_chemical_formula_weight         1018.19
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-05-16
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.862(2)
_cell_length_b                   19.608(4)
_cell_length_c                   26.579(5)
_cell_measurement_reflns_used    4356
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     6703(2)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            32751
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.53
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.405
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    2.018
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3936
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.013
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         5909
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.269
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+9.3985P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1345
_refine_ls_wR_factor_ref         0.1626
_reflns_number_gt                3346
_reflns_number_total             5909
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40672e.txt
_cod_data_source_block           3
_cod_database_code               7210291
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\sim As1: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
F4 \\sim F5 \\sim F6: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
F11 \\sim F7 \\sim F12 \\sim F8 \\sim F9 \\sim F10: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
F5 \\sim F4 \\sim F6 \\sim As2: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F6) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C11(H11A,
 H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C)
;