Solvent-assisted solid-state synthesis: separating the chemical from the mechanical in mechanochemical synthesis.
Bowmaker, Graham A; Hanna, John V; Skelton, Brian W; White, Allan H; Chemical communications (Cambridge, England) 34 (2009) 2168–2170; doi:10.1039/b822370j

data_7104327
_publ_section_title
;
 Solvent-assisted solid-state synthesis: separating the chemical from
 the mechanical in mechanochemical synthesis.
;
_journal_issue                   16
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2168
_journal_page_last               2170
_journal_paper_doi               10.1039/b822370j
_journal_volume                  34
_journal_year                    2009
_chemical_formula_moiety         'C7 H12 Cu N5 S3'
_chemical_formula_sum            'C7 H12 Cu N5 S3'
_chemical_formula_weight         325.94
_chemical_name_systematic
;
?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2008-11-07T13:23:37-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.484(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.0213(2)
_cell_length_b                   14.5533(4)
_cell_length_c                   7.1466(2)
_cell_measurement_reflns_used    4667
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.7262
_cell_measurement_theta_min      3.2322
_cell_volume                     611.45(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type
;
Oxford Diffraction Gemini diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0012366487
_diffrn_orient_matrix_UB_12      0.0395116911
_diffrn_orient_matrix_UB_13      0.0584325662
_diffrn_orient_matrix_UB_21      0.1204857829
_diffrn_orient_matrix_UB_22      -0.0007102927
_diffrn_orient_matrix_UB_23      0.0222861591
_diffrn_orient_matrix_UB_31      0.0014186896
_diffrn_orient_matrix_UB_32      0.0285756592
_diffrn_orient_matrix_UB_33      -0.0800366948
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10048
_diffrn_reflns_theta_full        33.5
_diffrn_reflns_theta_max         34.89
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    2.277
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.77
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.97
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         2625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.97
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0632
_reflns_number_gt                2007
_reflns_number_total             2625
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b822370j.txt
_cod_data_source_block           gb0898
_cod_original_sg_symbol_Hall     -P_2yb
_cod_database_code               7104327