#------------------------------------------------------------------------------
#$Date: 2019-11-23 04:20:41 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232101 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/69/4346999.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4346999
loop_
_publ_author_name
'Becker, Sabine'
'Dürr, Maximilian'
'Miska, Andreas'
'Becker, Jonathan'
'Gawlig, Christopher'
'Behrens, Ulrich'
'Ivanović-Burmazović, Ivana'
'Schindler, Siegfried'
_publ_section_title
;
 Copper Chloride Catalysis: Do μ4-Oxido Copper Clusters Play a
 Significant Role?
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3759
_journal_page_last               3766
_journal_paper_doi               10.1021/acs.inorgchem.5b02576
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C4 H12 Cl2 Cu O2 S2'
_chemical_formula_weight         290.70
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-03-02 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9620(16)
_cell_length_b                   11.483(2)
_cell_length_c                   11.325(2)
_cell_measurement_reflns_used    387
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.00
_cell_volume                     1035.4(3)
_computing_cell_refinement
;
 Denzo/Scalepack (HKL Research, Inc., 1997)

;
_computing_data_collection       'Bruker AXS Collect (2009)'
_computing_data_reduction
;
 Denzo/Scalepack (HKL Research, Inc., 1997)

;
_computing_molecular_graphics    'ShelXle (Huebschle, 2014)'
_computing_publication_material  'Ortep 3v2'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      190(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4534
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.516
_diffrn_reflns_theta_min         2.526
_diffrn_source                   'Bruker Nonius FR591 rotating anode'
_exptl_absorpt_coefficient_mu    2.982
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.865
_exptl_crystal_description       plate
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.0073(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         1247
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0229
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0230P)²+0.4878P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0566
_refine_ls_wR_factor_ref         0.0588
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1096
_reflns_number_total             1247
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b02576_si_004.cif
_cod_data_source_block           schindler13080
_cod_original_cell_volume        1035.4(4)
_cod_database_code               4346999
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.229
_shelx_estimated_absorpt_t_max   0.796
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.17761(4) 0.7500 0.36130(3) 0.01647(13) Uani 1 2 d S T P
O1 O 0.18373(14) 0.58047(12) 0.35274(12) 0.0199(3) Uani 1 1 d . . .
S1 S 0.31963(5) 0.51722(4) 0.42435(4) 0.01794(14) Uani 1 1 d . . .
Cl1 Cl 0.19997(9) 0.7500 0.56207(6) 0.02458(18) Uani 1 2 d S T P
C1 C 0.2066(3) 0.4165(2) 0.5120(2) 0.0324(5) Uani 1 1 d . . .
H1A H 0.1337 0.3693 0.4613 0.049 Uiso 1 1 calc R U .
H1B H 0.1379 0.4587 0.5696 0.049 Uiso 1 1 calc R U .
H1C H 0.2856 0.3656 0.5537 0.049 Uiso 1 1 calc R U .
C2 C 0.4110(3) 0.42112(18) 0.3209(2) 0.0303(5) Uani 1 1 d . . .
H2A H 0.3223 0.3775 0.2804 0.045 Uiso 1 1 calc R U .
H2B H 0.4856 0.3667 0.3620 0.045 Uiso 1 1 calc R U .
H2C H 0.4757 0.4659 0.2629 0.045 Uiso 1 1 calc R U .
Cl2 Cl -0.00014(7) 0.7500 0.20266(6) 0.02210(17) Uani 1 2 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Cu1 O1 173.62(8) 7_575 .
O1 Cu1 Cl1 92.73(4) 7_575 .
O1 Cu1 Cl1 92.73(4) . .
O1 Cu1 Cl2 88.65(4) 7_575 .
O1 Cu1 Cl2 88.65(4) . .
Cl1 Cu1 Cl2 146.25(3) . .
O1 Cu1 Cl2 87.85(4) 7_575 6_656
O1 Cu1 Cl2 87.85(4) . 6_656
Cl1 Cu1 Cl2 101.29(3) . 6_656
Cl2 Cu1 Cl2 112.46(2) . 6_656
S1 O1 Cu1 117.63(7) . .
O1 S1 C2 103.62(9) . .
O1 S1 C1 104.30(9) . .
C2 S1 C1 99.97(11) . .
Cu1 Cl2 Cu1 144.00(3) . 6_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.9498(14) 7_575
Cu1 O1 1.9498(14) .
Cu1 Cl1 2.2806(9) .
Cu1 Cl2 2.2871(7) .
Cu1 Cl2 2.6660(8) 6_656
O1 S1 1.5348(13) .
S1 C2 1.766(2) .
S1 C1 1.770(2) .
Cl2 Cu1 2.6660(8) 6_556
