Unexpected multiple bond cleavage and rearrangement of organosulfide ligands in the presence of Cu(II) assisted by solvothermal and solvothermal-microwave conditions.
Delgado, Salomé; Gallego, Almudena; Castillo, Oscar; Zamora, Félix; Dalton transactions (Cambridge, England : 2003) 40 (2011) 847–852; doi:10.1039/c0dt00973c

data_7014586
_publ_section_title
;
 Unexpected multiple bond cleavage and rearrangement of organosulfide
 ligands in the presence of Cu(II) assisted by solvothermal and
 solvothermal-microwave conditions.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              847
_journal_page_last               852
_journal_paper_doi               10.1039/c0dt00973c
_journal_volume                  40
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C16 H12 Cl4 Cu2 N8 S5.80'
_chemical_formula_structural     'C16 H12 Cl4 Cu2 N8 S5.80'
_chemical_formula_sum            'C16 H12 Cl4 Cu2 N8 S5.8'
_chemical_formula_weight         771.11
_chemical_name_systematic
;
poly-[mu-chlorido-(mu-bis(2-pyrimidyl-disulfide-k2N:N')copper(I)]-methanol
(1/1)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.541(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.9670(6)
_cell_length_b                   6.8657(4)
_cell_length_c                   16.9169(8)
_cell_measurement_reflns_used    20691
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.72
_cell_measurement_theta_min      2.58
_cell_volume                     1301.55(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir92 (Altamore et al., 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20691
_diffrn_reflns_theta_full        29.72
_diffrn_reflns_theta_max         29.72
_diffrn_reflns_theta_min         2.58
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.553
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++)
(compiled Jun 6 2003,13:53:32)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.984
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             765.5
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         3681
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0345P)^2^+5.4377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1189
_reflns_number_gt                3144
_reflns_number_total             3681
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT00973C.TXT
_cod_data_source_block           compound-2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C16 H12 Cl4 Cu2 N8 S5.80'
_cod_database_code               7014586