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_7210290
_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
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_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         'C12 H12 Ag2 F6 N4 O4 S2'
_chemical_formula_sum            'C12 H12 Ag2 F6 N4 O4 S2'
_chemical_formula_weight         670.12
_chemical_name_systematic
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 ? 
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_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_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                70.620(2)
_cell_angle_beta                 79.114(2)
_cell_angle_gamma                74.141(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9829(13)
_cell_length_b                   11.1316(16)
_cell_length_c                   11.1548(16)
_cell_measurement_reflns_used    2914
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.73
_cell_volume                     1006.2(3)
_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.
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_computing_publication_material
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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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5185
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.95
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.235
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0999 before and 0.0286 after correction.
The Ratio of minimum to maximum transmission is 0.8224.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    2.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.704
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.0448(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         3528
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0412P)^2^+1.4891P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                3122
_reflns_number_total             3528
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40672e.txt
_cod_data_source_block           2
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_database_code               7210290
_olex2_refinement_description
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1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F4-C12 = F5-C12 = F6-C12 = F4'-C12 = F5'-C12 = F6'-C12
 1.35 with sigma of 0.01
 O3-O4 = O2B-O1A
 2.2 with sigma of 0.01
 O1B-O2A
 2.2 with sigma of 0.01
 F4-F5 \\sim F4-F6 \\sim F5-F6
 with sigma of 0.001
 F4'-F5' \\sim F4'-F6' \\sim F5'-F6'
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
F2B \\sim F2A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1B) \\sim Ueq, Uanis(O1A) \\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(O2B) \\sim Ueq, Uanis(F2B) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F3B) \\sim Ueq, Uanis(F1B) \\sim Ueq, Uanis(F1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F4') \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F5') \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6') \\sim Ueq, Uanis(F6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1A) = Uanis(O1B)
Uanis(O2A) = Uanis(O2B)
4. Others
 Sof(F4')=Sof(F5')=Sof(F6')=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(O1B)=Sof(O2B)=1-FVAR(2)
 Sof(O2A)=Sof(O1A)=Sof(F2A)=Sof(F1A)=Sof(F3A)=FVAR(2)
5.a Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;