Solvent-assisted mechanochemical synthesis of metal complexes
Bowmaker, Graham A.; Chaichit, Narongsak; Pakawatchai, Chaveng; Skelton, Brian W.; White, Allan H.; Dalton Transactions  (2008) 2926–2928; doi:10.1039/b804229m

data_7004204
_publ_section_title
;
 Solvent-assisted mechanochemical synthesis of metal complexes
;
_journal_issue                   22
_journal_name_full               'Dalton Transactions'
_journal_page_first              2926
_journal_page_last               2928
_journal_paper_doi               10.1039/b804229m
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C9 H18 Ag Cl N6 S3'
_chemical_formula_sum            'C9 H18 Ag Cl N6 S3'
_chemical_formula_weight         449.79
_chemical_name_systematic
;
?
;
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2007-12-28T18:52:51-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   14.73800(10)
_cell_length_b                   14.73800(10)
_cell_length_c                   12.29650(10)
_cell_measurement_reflns_used    40774
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      43.4143
_cell_measurement_theta_min      3.5863
_cell_volume                     2313.07(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
Oxford Diffraction Gemini diffractometer
;
_diffrn_measurement_method       '\p and \w scans'
_diffrn_orient_matrix_UB_11      -0.015512104
_diffrn_orient_matrix_UB_12      -0.0409384497
_diffrn_orient_matrix_UB_13      -0.0384939749
_diffrn_orient_matrix_UB_21      0.0391317434
_diffrn_orient_matrix_UB_22      -0.0102934319
_diffrn_orient_matrix_UB_23      0.0199144611
_diffrn_orient_matrix_UB_31      -0.0362594086
_diffrn_orient_matrix_UB_32      -0.0361277508
_diffrn_orient_matrix_UB_33      0.0380050088
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0076
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49899
_diffrn_reflns_theta_full        43.53
_diffrn_reflns_theta_max         43.53
_diffrn_reflns_theta_min         3.68
_exptl_absorpt_coefficient_mu    1.885
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.81196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.937
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.296
_refine_diff_density_min         -1.219
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.016(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         3907
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0157
_refine_ls_R_factor_gt           0.0152
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+0.9510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0367
_refine_ls_wR_factor_ref         0.037
_reflns_number_gt                3807
_reflns_number_total             3907
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b804229m.txt
_cod_data_source_block           gb0777
_cod_original_sg_symbol_Hall     r_3_-2"c
_cod_original_sg_symbol_H-M      R_3_c:h
_cod_database_code               7004204