#------------------------------------------------------------------------------
#$Date: 2019-11-23 04:20:25 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232100 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/69/4346998.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_4346998
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 H16 Cl3 Cu N2'
_chemical_formula_weight         262.08
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                113.14(3)
_cell_angle_beta                 100.38(3)
_cell_angle_gamma                100.33(3)
_cell_formula_units_Z            2
_cell_length_a                   7.2930(15)
_cell_length_b                   9.0060(18)
_cell_length_c                   9.6850(19)
_cell_measurement_reflns_used    216
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.00
_cell_volume                     552.9(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, 2015)'
_computing_publication_material  'Ortep 3v2'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_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_source         'Bruker Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7665
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.380
_exptl_absorpt_coefficient_mu    2.644
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5016
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             268
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0253
_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)+(0.0192P)²+0.3168P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0607
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1969
_reflns_number_total             2257
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b02576_si_008.cif
_cod_data_source_block           schindler12113
_cod_original_cell_volume        553.0(2)
_cod_database_code               4346998
_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   0.259
_shelx_estimated_absorpt_t_max   0.558
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
C1 C 0.4900(4) 0.1825(4) 0.6969(3) 0.0495(6) Uani 1 1 d
C2 C 0.1683(4) 0.2375(4) 0.6843(3) 0.0482(6) Uani 1 1 d
C3 C 0.9190(4) 0.3497(4) 0.1015(3) 0.0480(6) Uani 1 1 d
C4 C 0.7607(4) 0.1022(3) 0.1292(4) 0.0533(6) Uani 1 1 d
Cl1 Cl 0.21919(7) 0.08194(6) 0.29358(5) 0.03452(12) Uani 1 1 d
Cl2 Cl 0.72985(7) 0.42898(7) 0.49783(6) 0.04065(14) Uani 1 1 d
Cl3 Cl 0.40283(8) 0.35478(6) 0.09959(5) 0.03913(13) Uani 1 1 d
Cu1 Cu 0.43331(4) 0.31373(4) 0.31806(3) 0.05399(12) Uani 1 1 d
H1 H 0.505(4) 0.200(3) 0.803(3) 0.054(7) Uiso 1 1 d
H2 H 0.614(5) 0.218(4) 0.679(3) 0.072(9) Uiso 1 1 d
H3 H 0.426(4) 0.063(4) 0.629(3) 0.053(7) Uiso 1 1 d
H4 H 0.342(4) 0.260(3) 0.565(3) 0.053(7) Uiso 1 1 d
H5 H 0.418(4) 0.389(4) 0.720(4) 0.066(9) Uiso 1 1 d
H6 H 0.090(4) 0.294(3) 0.647(3) 0.052(7) Uiso 1 1 d
H7 H 0.181(4) 0.273(3) 0.797(4) 0.065(8) Uiso 1 1 d
H8 H 0.108(4) 0.121(4) 0.632(4) 0.068(9) Uiso 1 1 d
H9 H 0.933(4) 0.273(4) 0.003(4) 0.082(10) Uiso 1 1 d
H10 H 1.020(4) 0.450(4) 0.153(3) 0.060(8) Uiso 1 1 d
H11 H 0.800(4) 0.383(3) 0.084(3) 0.050(7) Uiso 1 1 d
H12 H 1.029(5) 0.260(4) 0.241(3) 0.071(9) Uiso 1 1 d
H13 H 0.889(4) 0.336(3) 0.295(3) 0.053(7) Uiso 1 1 d
H14 H 0.785(4) 0.029(4) 0.033(4) 0.079(10) Uiso 1 1 d
H15 H 0.632(4) 0.125(4) 0.111(3) 0.065(8) Uiso 1 1 d
H16 H 0.758(5) 0.061(4) 0.203(4) 0.083(11) Uiso 1 1 d
N1 N 0.3611(3) 0.2786(2) 0.6603(2) 0.0394(4) Uani 1 1 d
N2 N 0.9094(3) 0.2662(2) 0.2046(2) 0.0401(4) Uani 1 1 d
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'
N N 0.0061 0.0033 '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
Cl3 Cu1 Cl1 115.39(4)
Cl3 Cu1 Cl2 117.39(3)
Cl1 Cu1 Cl2 122.04(4)
C2 N1 C1 114.3(2)
C3 N2 C4 112.8(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N1 1.474(3)
C2 N1 1.472(3)
C3 N2 1.471(3)
C4 N2 1.477(3)
Cl1 Cu1 2.2719(10)
Cl2 Cu1 2.2814(12)
Cl3 Cu1 2.2667(7)
