#------------------------------------------------------------------------------
#$Date: 2019-11-23 04:20:55 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232103 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/70/4347000.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_4347000
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 H6 Cl6 Cu3 N2'
_chemical_formula_weight         485.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 105.91(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.737(2)
_cell_length_b                   6.1293(15)
_cell_length_c                   16.438(6)
_cell_measurement_reflns_used    1502
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      1.00
_cell_volume                     652.8(4)
_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, 2015)'
_computing_publication_material  'Ortep 3v2'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      190(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9662
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.022
_diffrn_reflns_theta_max         25.022
_diffrn_reflns_theta_min         3.144
_diffrn_source                   'Bruker Nonius FR591 rotating anode'
_exptl_absorpt_coefficient_mu    6.035
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.470
_exptl_crystal_description       block
_exptl_crystal_F_000             466
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       0.0035(6)
_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   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         1152
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0209
_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)+0.9296P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0459
_refine_ls_wR_factor_ref         0.0467
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1076
_reflns_number_total             1152
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b02576_si_007.cif
_cod_data_source_block           schindler12106
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4347000
_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   0.196
_shelx_estimated_absorpt_t_max   0.378
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.74096(5) 0.55587(5) 0.45694(2) 0.01572(13) Uani 1 1 d . . .
Cu2 Cu 0.5000 1.0000 0.5000 0.01918(15) Uani 1 2 d S . P
Cl1 Cl 0.88841(9) 0.26391(10) 0.53444(4) 0.01853(17) Uani 1 1 d . . .
Cl2 Cl 0.55906(9) 0.84421(10) 0.38263(4) 0.01738(17) Uani 1 1 d . . .
Cl3 Cl 0.67336(10) 0.71336(10) 0.57354(4) 0.01707(16) Uani 1 1 d . . .
N1 N 0.7547(4) 0.3987(4) 0.35298(14) 0.0208(5) Uani 1 1 d . . .
C1 C 0.7960(4) 0.2671(4) 0.31206(16) 0.0203(6) Uani 1 1 d . . .
C2 C 0.8565(5) 0.0956(5) 0.26340(18) 0.0288(7) Uani 1 1 d . . .
H1B H 0.9800 0.0222 0.2982 0.043 Uiso 1 1 calc R U .
H2A H 0.8867 0.1585 0.2133 0.043 Uiso 1 1 calc R U .
H3C H 0.7439 -0.0104 0.2457 0.043 Uiso 1 1 calc R U .
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'
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'
N N 0.0061 0.0033 '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
N1 Cu1 Cl1 89.09(7) . .
N1 Cu1 Cl3 170.81(7) . .
Cl1 Cu1 Cl3 91.11(3) . .
N1 Cu1 Cl2 93.40(7) . .
Cl1 Cu1 Cl2 173.73(3) . .
Cl3 Cu1 Cl2 85.51(3) . .
N1 Cu1 Cl1 89.02(7) . 3_766
Cl1 Cu1 Cl1 92.13(3) . 3_766
Cl3 Cu1 Cl1 100.15(3) . 3_766
Cl2 Cu1 Cl1 93.67(3) . 3_766
Cl3 Cu2 Cl3 180.0 3_676 .
Cl3 Cu2 Cl2 93.28(3) 3_676 .
Cl3 Cu2 Cl2 86.72(3) . .
Cl3 Cu2 Cl2 86.72(3) 3_676 3_676
Cl3 Cu2 Cl2 93.28(3) . 3_676
Cl2 Cu2 Cl2 180.00(3) . 3_676
Cu1 Cl1 Cu1 87.87(3) . 3_766
Cu2 Cl2 Cu1 93.64(3) . .
Cu2 Cl3 Cu1 94.11(3) . .
C1 N1 Cu1 159.0(2) . .
N1 C1 C2 177.2(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 1.986(2) .
Cu1 Cl1 2.2624(8) .
Cu1 Cl3 2.3003(9) .
Cu1 Cl2 2.3014(8) .
Cu1 Cl1 2.6984(10) 3_766
Cu2 Cl3 2.2667(8) 3_676
Cu2 Cl3 2.2667(8) .
Cu2 Cl2 2.2833(9) .
Cu2 Cl2 2.2833(9) 3_676
Cl1 Cu1 2.6984(10) 3_766
N1 C1 1.133(4) .
C1 C2 1.446(4) .
