#------------------------------------------------------------------------------
#$Date: 2019-11-23 00:20:20 +0200 (Sat, 23 Nov 2019) $
#$Revision: 231646 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/61/4346180.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_4346180
loop_
_publ_author_name
'Cherutoi, Jackson K.'
'Sandifer, Jace D.'
'Pokharel, Uttam R.'
'Fronczek, Frank R.'
'Pakhomova, Svetlana'
'Maverick, Andrew W.'
_publ_section_title
;
 Externally and Internally Functionalized Copper(II) β-Diketonate
 Molecular Squares.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7791
_journal_page_last               7802
_journal_paper_doi               10.1021/acs.inorgchem.5b00792
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C68 H72 Cu4 O20, 12(C H Cl3), O10'
_chemical_formula_sum            'C80 H84 Cl36 Cu4 O30'
_chemical_formula_weight         3055.82
_chemical_name_common
;
 tetrakis(5-methoxy-1,3-phenylenebis(acetylacetonato))diaquatetracopper
 chloroform-water solvate
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.366(5)
_cell_length_b                   19.366(5)
_cell_length_c                   19.977(5)
_cell_measurement_reflns_used    2671
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      22.986
_cell_measurement_theta_min      2.546
_cell_volume                     7492(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR97 (Altomare  et al., 1999)'
_diffrn_ambient_temperature      90.0(5)
_diffrn_measured_fraction_theta_full 0.764
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       'φ and ω scans '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.764
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4890
_diffrn_reflns_point_group_measured_fraction_full 0.764
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         22.992
_diffrn_reflns_theta_min         2.563
_exptl_absorpt_coefficient_mu    1.257
_exptl_absorpt_correction_T_max  0.7481
_exptl_absorpt_correction_T_min  0.6516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3064
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.365
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         2686
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0949
_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)+(0.1570P)²+90.5226P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2620
_refine_ls_wR_factor_ref         0.2701
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2282
_reflns_number_total             2686
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b00792_si_002.cif
_cod_data_source_block           cpd11_Jace1
_cod_original_cell_volume        7492(4)
_cod_database_code               4346180
_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   0.660
_shelx_estimated_absorpt_t_max   0.770
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.35181(6) 0.83878(6) 0.5000 0.0322(5) Uani 1 2 d S T P . .
O1 O 0.4138(2) 0.8665(3) 0.5686(2) 0.0374(12) Uani 1 1 d . . . . .
O2 O 0.8076(3) 0.7090(2) 0.4313(3) 0.0403(13) Uani 1 1 d . . . . .
O3 O 0.7119(3) 1.0426(4) 0.5000 0.049(2) Uani 1 2 d S T P . .
C1 C 0.5156(5) 0.8930(6) 0.6259(5) 0.063(3) Uani 1 1 d . . . . .
H1A H 0.5616 0.9117 0.6166 0.094 Uiso 1 1 calc R U . . .
H1B H 0.5201 0.8490 0.6499 0.094 Uiso 1 1 calc R U . . .
H1C H 0.4897 0.9258 0.6536 0.094 Uiso 1 1 calc R U . . .
C2 C 0.4781(3) 0.8815(4) 0.5617(4) 0.0353(17) Uani 1 1 d . . . . .
C3 C 0.5119(5) 0.8888(5) 0.5000 0.031(2) Uani 1 2 d S T P . .
C4 C 0.5882(5) 0.9013(5) 0.5000 0.035(2) Uani 1 2 d S T P . .
C5 C 0.6166(5) 0.9674(5) 0.5000 0.037(2) Uani 1 2 d S T P . .
H5 H 0.5872 1.0066 0.5000 0.044 Uiso 1 2 calc R U P . .
C6 C 0.6883(5) 0.9764(5) 0.5000 0.039(3) Uani 1 2 d S T P . .
C7 C 0.7319(5) 0.9190(5) 0.5000 0.034(2) Uani 1 2 d S T P . .
H7 H 0.7805 0.9251 0.5000 0.041 Uiso 1 2 calc R U P . .
C8 C 0.7038(5) 0.8525(5) 0.5000 0.035(2) Uani 1 2 d S T P . .
C9 C 0.6330(5) 0.8449(5) 0.5000 0.038(2) Uani 1 2 d S T P . .
H9 H 0.6141 0.7996 0.5000 0.046 Uiso 1 2 calc R U P . .
C10 C 0.7475(5) 0.7964(5) 0.3743(5) 0.062(3) Uani 1 1 d . . . . .
H10A H 0.7615 0.7676 0.3363 0.094 Uiso 1 1 calc R U . . .
H10B H 0.7694 0.8419 0.3706 0.094 Uiso 1 1 calc R U . . .
H10C H 0.6972 0.8019 0.3740 0.094 Uiso 1 1 calc R U . . .
C11 C 0.7694(4) 0.7627(4) 0.4382(4) 0.0407(18) Uani 1 1 d . . . . .
C12 C 0.7501(5) 0.7915(5) 0.5000 0.033(2) Uani 1 2 d S T P . .
C13 C 0.7855(6) 1.0518(5) 0.5000 0.061(4) Uani 1 2 d S T P . .
H13A H 0.7963 1.1013 0.5000 0.091 Uiso 1 2 calc R U P . .
H13B H 0.8052 1.0303 0.4599 0.091 Uiso 0.5 1 calc R U P . .
H13C H 0.8052 1.0303 0.5401 0.091 Uiso 0.5 1 calc R U P . .
Cl1 Cl 0.49652(15) 0.84090(17) 0.81292(15) 0.0842(10) Uani 1 1 d D . . . .
Cl2 Cl 0.63454(16) 0.8311(2) 0.76188(15) 0.0938(11) Uani 1 1 d D . . . .
Cl3 Cl 0.5661(2) 0.71131(17) 0.8169(3) 0.1338(18) Uani 1 1 d D . . . .
C1S C 0.5773(5) 0.8008(5) 0.8204(5) 0.065(3) Uani 1 1 d D . . . .
H1S H 0.5962 0.8124 0.8657 0.078 Uiso 1 1 calc R U . . .
C2S C 0.7060(8) 0.5922(6) 0.6377(6) 0.068(4) Uani 0.5 1 d D U P . .
H20 H 0.7546 0.6094 0.6359 0.081 Uiso 0.5 1 calc R U P A 1
Cl4 Cl 0.6714(8) 0.6148(9) 0.5613(7) 0.088(5) Uani 0.192(8) 1 d D U P B 1
Cl5 Cl 0.7142(11) 0.5028(7) 0.6445(9) 0.076(5) Uani 0.192(8) 1 d D U P B 1
Cl6 Cl 0.6724(8) 0.6306(8) 0.7043(8) 0.075(5) Uani 0.192(8) 1 d D U P B 1
Cl7 Cl 0.6356(5) 0.6421(5) 0.6043(6) 0.088(3) Uani 0.308(8) 1 d D U P B 2
Cl8 Cl 0.6956(9) 0.5063(7) 0.6159(11) 0.120(5) Uani 0.308(8) 1 d D U P B 2
Cl9 Cl 0.6919(8) 0.5989(11) 0.7242(6) 0.132(5) Uani 0.308(8) 1 d D U P B 2
O1W O 0.5852(7) 0.5554(6) 0.8860(10) 0.211(8) Uani 1 1 d . U . . .
O2W O 0.7138(14) 0.5927(16) 0.5000 0.132(11) Uani 0.5 2 d S TU 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'
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'
O O 0.0106 0.0060 '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 92.3(3) . 10_556
O1 Cu1 O2 177.9(2) . 3_655
O1 Cu1 O2 87.8(2) 10_556 3_655
O1 Cu1 O2 87.8(2) . 12_656
O1 Cu1 O2 177.9(2) 10_556 12_656
O2 Cu1 O2 92.1(3) 3_655 12_656
C2 O1 Cu1 126.8(5) . .
C11 O2 Cu1 127.3(5) . 11_566
C6 O3 C13 116.7(8) . .
C2 C1 H1A 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
O1 C2 C3 124.7(7) . .
O1 C2 C1 114.4(7) . .
C3 C2 C1 120.9(6) . .
C2 C3 C2 122.9(8) . 10_556
C2 C3 C4 118.5(4) . .
C2 C3 C4 118.5(4) 10_556 .
C5 C4 C9 118.3(9) . .
C5 C4 C3 122.5(9) . .
C9 C4 C3 119.2(9) . .
C4 C5 C6 120.4(9) . .
C4 C5 H5 119.8 . .
C6 C5 H5 119.8 . .
O3 C6 C7 123.3(9) . .
O3 C6 C5 116.7(8) . .
C7 C6 C5 120.0(9) . .
C6 C7 C8 119.9(9) . .
C6 C7 H7 120.0 . .
C8 C7 H7 120.0 . .
C9 C8 C7 119.0(9) . .
C9 C8 C12 121.1(9) . .
C7 C8 C12 119.9(8) . .
C8 C9 C4 122.3(10) . .
C8 C9 H9 118.8 . .
C4 C9 H9 118.8 . .
C11 C10 H10A 109.5 . .
C11 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C11 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
O2 C11 C12 124.7(7) . .
O2 C11 C10 115.2(7) . .
C12 C11 C10 120.1(7) . .
C11 C12 C11 122.9(9) . 10_556
C11 C12 C8 118.5(4) . .
C11 C12 C8 118.5(4) 10_556 .
O3 C13 H13A 109.5 . .
O3 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
O3 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
Cl2 C1S Cl3 113.0(5) . .
Cl2 C1S Cl1 111.6(5) . .
Cl3 C1S Cl1 108.9(5) . .
Cl2 C1S H1S 107.7 . .
Cl3 C1S H1S 107.7 . .
Cl1 C1S H1S 107.7 . .
Cl6 C2S Cl4 116.3(10) . .
Cl6 C2S Cl5 114.8(11) . .
Cl4 C2S Cl5 110.9(10) . .
Cl8 C2S Cl9 107.6(11) . .
Cl8 C2S Cl7 109.6(10) . .
Cl9 C2S Cl7 102.0(9) . .
Cl6 C2S H20 104.4 . .
Cl4 C2S H20 104.4 . .
Cl5 C2S H20 104.4 . .
O2W Cl4 C2S 115.3(13) . .
Cl4 O2W Cl4 105.9(18) . 10_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.899(5) .
Cu1 O1 1.899(5) 10_556
Cu1 O2 1.906(5) 3_655
Cu1 O2 1.906(5) 12_656
O1 C2 1.285(8) .
O2 C11 1.284(9) .
O2 Cu1 1.906(5) 11_566
O3 C6 1.360(12) .
O3 C13 1.437(13) .
C1 C2 1.492(11) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 C3 1.403(9) .
C3 C2 1.403(9) 10_556
C3 C4 1.497(13) .
C4 C5 1.394(14) .
C4 C9 1.395(14) .
C5 C6 1.399(14) .
C5 H5 0.9500 .
C6 C7 1.395(14) .
C7 C8 1.399(14) .
C7 H7 0.9500 .
C8 C9 1.378(15) .
C8 C12 1.483(14) .
C9 H9 0.9500 .
C10 C11 1.497(12) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 C12 1.405(9) .
C12 C11 1.405(9) 10_556
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
Cl1 C1S 1.753(9) .
Cl2 C1S 1.714(10) .
Cl3 C1S 1.749(9) .
C1S H1S 1.0000 .
C2S Cl6 1.658(15) .
C2S Cl4 1.723(14) .
C2S Cl8 1.731(16) .
C2S Cl5 1.743(15) .
C2S Cl9 1.753(15) .
C2S Cl7 1.800(14) .
C2S H20 1.0000 .
Cl4 O2W 1.54(2) .
Cl4 Cl4 2.45(3) 10_556
O2W Cl4 1.54(2) 10_556
