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#$Date: 2019-11-23 04:21:07 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232104 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/70/4347001.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_4347001
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            'C1.5 H5 Cl2 Cu O1.5'
_chemical_formula_weight         181.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-03-02 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 93.88(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.836(4)
_cell_length_b                   3.2840(7)
_cell_length_c                   9.5930(19)
_cell_measurement_reflns_used    220
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.00
_cell_volume                     560.6(2)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0540
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1775
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        24.976
_diffrn_reflns_theta_max         24.976
_diffrn_reflns_theta_min         3.019
_diffrn_source                   'Bruker Nonius FR591 rotating anode'
_exptl_absorpt_coefficient_mu    4.713
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.150
_exptl_crystal_description       needle
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         577
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0178P)²+6.4514P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1101
_reflns_Friedel_coverage         0.000
_reflns_number_gt                490
_reflns_number_total             577
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b02576_si_002.cif
_cod_data_source_block           schindler13114
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_original_formula_sum        'C1.50 H5 Cl2 Cu O1.50'
_cod_database_code               4347001
_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   0.202
_shelx_estimated_absorpt_t_max   0.954
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.83479(6) 0.0000 0.39272(11) 0.0215(4) Uani 1 2 d DS T P
Cl1 Cl 0.84117(12) 0.5000 0.5584(2) 0.0244(5) Uani 1 2 d S T P
Cl2 Cl 0.81075(13) 0.5000 0.2316(2) 0.0258(6) Uani 1 2 d S T P
O1 O 0.9617(4) 0.0000 0.3718(7) 0.048(2) Uani 1 2 d DS T P
H1 H 0.9836(17) 0.0000 0.297(2) 0.10(4) Uiso 1 2 d DS U P
H2 H 0.9957(14) 0.0000 0.436(3) 0.10(4) Uiso 1 2 d DS U P
O2 O 1.0139(7) 0.5000 0.1907(15) 0.033(3) Uani 0.5 2 d S T P
C1 C 1.0700(11) 0.5000 0.125(2) 0.029(4) Uani 0.5 2 d S T P
C2 C 1.1076(9) 0.886(4) 0.0903(15) 0.041(4) Uani 0.5 1 d . . P
H2A H 1.1232 0.8738 -0.0057 0.062 Uiso 0.5 1 calc R U P
H2B H 1.1518 0.9273 0.1550 0.062 Uiso 0.5 1 calc R U P
H2C H 1.0726 1.1138 0.0988 0.062 Uiso 0.5 1 calc R U 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'
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
Cl2 Cu1 Cl2 92.34(9) 1_545 .
Cl2 Cu1 Cl1 171.93(9) 1_545 .
Cl2 Cu1 Cl1 87.26(6) . .
Cl2 Cu1 Cl1 87.26(6) 1_545 1_545
Cl2 Cu1 Cl1 171.93(9) . 1_545
Cl1 Cu1 Cl1 92.01(9) . 1_545
Cl2 Cu1 O1 94.73(13) 1_545 .
Cl2 Cu1 O1 94.73(14) . .
Cl1 Cu1 O1 93.34(14) . .
Cl1 Cu1 O1 93.34(14) 1_545 .
Cu1 Cl1 Cu1 92.01(9) 1_565 .
Cu1 Cl2 Cu1 92.34(9) 1_565 .
Cu1 O1 H1 127(2) . .
Cu1 O1 H2 127(2) . .
H1 O1 H2 106(3) . .
O2 C1 C2 121.0(9) . .
O2 C1 C2 121.0(9) . 6_565
C2 C1 C2 117.7(17) . 6_565
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 Cl2 2.2761(18) 1_545
Cu1 Cl2 2.2761(18) .
Cu1 Cl1 2.2825(18) .
Cu1 Cl1 2.2825(18) 1_545
Cu1 O1 2.286(7) .
Cl1 Cu1 2.2825(18) 1_565
Cl2 Cu1 2.2761(18) 1_565
O1 H1 0.837(10) .
O1 H2 0.836(10) .
O2 C1 1.22(2) .
C1 C2 1.483(16) .
C1 C2 1.483(16) 6_565
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
