N2O reduction at a dissymmetric {Cu2S}-containing mixed-valent center
Esmieu, Charlène; Orio, Maylis; Torelli, Stéphane; Le Pape, Laurent; Pécaut, Jacques; Lebrun, Colette; Ménage, Stéphane; Chem. Sci. 5 (2014) 4774–; doi:10.1039/C4SC01487A

data_1517286
_publ_section_title
;
 N2O reduction at a dissymmetric {Cu2S}-containing mixed-valent center
;
_journal_issue                   12
_journal_name_full               'Chem. Sci.'
_journal_page_first              4774
_journal_paper_doi               10.1039/C4SC01487A
_journal_volume                  5
_journal_year                    2014
_chemical_formula_sum            'C19 H26 O5 S2'
_chemical_formula_weight         398.52
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.759(5)
_cell_angle_beta                 72.017(5)
_cell_angle_gamma                78.159(5)
_cell_formula_units_Z            2
_cell_length_a                   8.5289(5)
_cell_length_b                   10.9789(7)
_cell_length_c                   11.4493(7)
_cell_measurement_reflns_used    2777
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.3829
_cell_measurement_theta_min      3.4792
_cell_volume                     997.68(11)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
  1 omega    4.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   77.0000 -150.0000 90

  2 omega  -94.00   -4.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000  -90.0000 90

  3 omega  -92.00   -3.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000    0.0000 89

  4 omega  -57.00   40.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   77.0000  120.0000 97

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.1063
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9120
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.49
_exptl_absorpt_coefficient_mu    0.293
_exptl_absorpt_correction_T_max  0.9724
_exptl_absorpt_correction_T_min  0.9283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.802
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         6009
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.802
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0265P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0768
_reflns_number_gt                3438
_reflns_number_total             6009
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sc01487a2.cif
_cod_data_source_block           st376
_cod_depositor_comments
'Adding full bibliography for 1517286--1517289.cif.'
_cod_database_code               1517286