#------------------------------------------------------------------------------
#$Date: 2025-08-04 10:03:09 +0300 (Mon, 04 Aug 2025) $
#$Revision: 301442 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/65/7056554.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_7056554
loop_
_publ_author_name
'Li, Xiaoqin'
'Ma, Dan'
'Cao, Bingran'
'Lu, Ying'
_publ_section_title
;
 Windmill-type mixed-metal clusters containing schiff-base ligands as
 efficient catalyst for cyclohexene oxidation
;
_journal_issue                   20
_journal_name_full               'New J. Chem.'
_journal_page_first              11619
_journal_page_last               11625
_journal_paper_doi               10.1039/C7NJ02359F
_journal_volume                  41
_journal_year                    2017
_chemical_formula_sum            'C84 H102 Cl6 Cu7 N12 O21 Zn2'
_chemical_formula_weight         2404.11
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-23 deposited with the CCDC.
2017-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   22.2759(3)
_cell_length_b                   22.2759(3)
_cell_length_c                   16.4697(6)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.2479
_cell_measurement_theta_min      2.6894
_cell_volume                     7077.6(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  bruker-CCd
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6049
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.055
_exptl_absorpt_coefficient_mu    2.289
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_description       block
_exptl_crystal_F_000             3668
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.617
_refine_diff_density_min         -3.235
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         2755
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0653
_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)+(0.0898P)²+115.7487P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1808
_refine_ls_wR_factor_ref         0.1934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2227
_reflns_number_total             2755
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7nj02359f2.cif
_cod_data_source_block           ee
_cod_database_code               7056554
#BEGIN Tags that were not found in dictionaries:
_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   0.645
_shelx_estimated_absorpt_t_max   0.670
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Zn1 Zn 0.0000 0.0000 0.23045(8) 0.0381(4) Uani 1 3 d S T P . .
Cu1 Cu -0.47250(4) -0.14083(4) 0.19860(5) 0.0390(3) Uani 1 1 d . . . . .
Cu2 Cu 0.0000 0.0000 0.0000 0.0548(6) Uani 1 6 d S T P . .
Cl1 Cl -0.55311(11) -0.16437(13) 0.09885(11) 0.0625(6) Uani 1 1 d . . . . .
O1 O -0.4057(2) -0.1272(3) 0.1177(3) 0.0459(12) Uani 1 1 d . . . . .
O2 O -0.0969(3) -0.0318(3) 0.2183(4) 0.0566(13) Uani 1 1 d . U . . .
O3 O -0.0885(3) -0.0270(4) 0.0851(4) 0.094(2) Uani 1 1 d . U . . .
N1 N -0.5366(3) -0.1447(3) 0.2858(3) 0.0436(13) Uani 1 1 d . . . . .
H1A H -0.5593 -0.1229 0.2690 0.052 Uiso 1 1 d R U . A .
H1B H -0.5681 -0.1891 0.2967 0.052 Uiso 1 1 d R U . . .
N2 N -0.4037(3) -0.1055(4) 0.2865(3) 0.0563(18) Uani 1 1 d . . . . .
C7 C -0.3397(4) -0.0877(4) 0.2801(4) 0.053(2) Uani 1 1 d . . . . .
H7 H -0.3133 -0.0747 0.3274 0.063 Uiso 1 1 calc R U . . .
C8 C -0.3053(3) -0.0863(4) 0.2055(4) 0.0397(15) Uani 1 1 d . . . . .
C9 C -0.2348(3) -0.0646(4) 0.2099(4) 0.0421(15) Uani 1 1 d . . . . .
H9 H -0.2131 -0.0534 0.2604 0.051 Uiso 1 1 calc R U . . .
C10 C -0.1966(3) -0.0593(4) 0.1428(4) 0.0446(16) Uani 1 1 d . . . . .
C11 C -0.2301(4) -0.0754(5) 0.0668(5) 0.059(2) Uani 1 1 d . . . . .
H11 H -0.2048 -0.0711 0.0201 0.071 Uiso 1 1 calc R U . . .
C12 C -0.2986(4) -0.0968(5) 0.0607(4) 0.057(2) Uani 1 1 d . . . . .
H12 H -0.3190 -0.1069 0.0095 0.069 Uiso 1 1 calc R U . . .
C13 C -0.3399(3) -0.1045(3) 0.1288(4) 0.0400(15) Uani 1 1 d . . . . .
C14 C -0.1222(4) -0.0377(4) 0.1488(5) 0.055(2) Uani 1 1 d . . . . .
O2W O 0.0000 0.0000 0.5000 0.124(5) Uani 1 6 d GS TU P . .
H2WB H -0.0480 -0.0164 0.5110 0.186 Uiso 0.1667 1 d R U P . .
H2WA H 0.0103 -0.0362 0.5110 0.186 Uiso 0.1667 1 d R U P . .
C1 C -0.4927(6) -0.1004(8) 0.3567(5) 0.030(3) Uani 0.512(16) 1 d D U P A 1
H1 H -0.4701 -0.0512 0.3420 0.036 Uiso 0.512(16) 1 calc R U P A 1
C2 C -0.5368(3) -0.1136(4) 0.4319(4) 0.0514(18) Uani 0.512(16) 1 d D U P A 1
H2A H -0.5545 -0.0817 0.4317 0.062 Uiso 0.512(16) 1 calc R U P A 1
H2B H -0.5763 -0.1602 0.4287 0.062 Uiso 0.512(16) 1 calc R U P A 1
C3 C -0.5008(6) -0.1061(12) 0.5102(6) 0.076(6) Uani 0.512(16) 1 d D U P A 1
H3A H -0.5085 -0.1512 0.5271 0.091 Uiso 0.512(16) 1 calc R U P A 1
H3B H -0.5203 -0.0897 0.5513 0.091 Uiso 0.512(16) 1 calc R U P A 1
C4 C -0.4245(6) -0.0568(11) 0.5043(10) 0.074(6) Uani 0.512(16) 1 d D U P A 1
H4A H -0.4030 -0.0565 0.5556 0.089 Uiso 0.512(16) 1 calc R U P A 1
H4B H -0.4168 -0.0105 0.4950 0.089 Uiso 0.512(16) 1 calc R U P A 1
C5 C -0.3899(3) -0.0748(5) 0.4370(4) 0.060(2) Uani 0.512(16) 1 d D U P A 1
H5A H -0.3549 -0.0321 0.4119 0.072 Uiso 0.512(16) 1 calc R U P A 1
H5B H -0.3664 -0.0973 0.4609 0.072 Uiso 0.512(16) 1 calc R U P A 1
C6 C -0.4383(5) -0.1214(6) 0.3716(6) 0.026(3) Uani 0.512(16) 1 d D U P A 1
H6 H -0.4592 -0.1706 0.3859 0.032 Uiso 0.512(16) 1 calc R U P A 1
C6A C -0.4281(5) -0.0800(9) 0.3590(6) 0.054(5) Uani 0.488(16) 1 d D U P A 2
H6A H -0.4218 -0.0342 0.3460 0.065 Uiso 0.488(16) 1 calc R U P A 2
C3A C -0.4870(6) -0.0689(8) 0.4990(7) 0.044(4) Uani 0.488(16) 1 d D U P A 2
H3AA H -0.4647 -0.0205 0.4833 0.053 Uiso 0.488(16) 1 calc R U P A 2
H3AB H -0.5128 -0.0746 0.5486 0.053 Uiso 0.488(16) 1 calc R U P A 2
C1A C -0.5041(6) -0.1313(9) 0.3634(8) 0.049(5) Uani 0.488(16) 1 d D U P A 2
H1AA H -0.5070 -0.1751 0.3794 0.059 Uiso 0.488(16) 1 calc R U P A 2
C4A C -0.4326(7) -0.0894(10) 0.5139(6) 0.051(5) Uani 0.488(16) 1 d D U P A 2
H4AA H -0.4547 -0.1382 0.5275 0.062 Uiso 0.488(16) 1 calc R U P A 2
H4AB H -0.4030 -0.0628 0.5588 0.062 Uiso 0.488(16) 1 calc R U P A 2
C2A C -0.5368(3) -0.1136(4) 0.4319(4) 0.0514(18) Uani 0.488(16) 1 d D U P A 2
H2AA H -0.5726 -0.1564 0.4559 0.062 Uiso 0.488(16) 1 calc R U P A 2
H2AB H -0.5592 -0.0894 0.4098 0.062 Uiso 0.488(16) 1 calc R U P A 2
C5A C -0.3899(3) -0.0748(5) 0.4370(4) 0.060(2) Uani 0.488(16) 1 d D U P A 2
H5AA H -0.3499 -0.0286 0.4408 0.072 Uiso 0.488(16) 1 calc R U P A 2
H5AB H -0.3729 -0.1072 0.4342 0.072 Uiso 0.488(16) 1 calc R U P A 2
O1W O 0.0195(14) 0.0302(10) 0.3544(12) 0.092(5) Uani 0.3333 1 d . U P . .
H1WA H 0.0509 0.0737 0.3688 0.138 Uiso 0.3333 1 d R U P . .
H1WC H -0.0065 -0.0061 0.3907 0.138 Uiso 0.3333 1 d 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 0.0030 0.0020 '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 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3200 1.2650 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2840 1.4300 '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
O2 Zn1 O2 118.93(6) . 3
O2 Zn1 O2 118.93(6) . 2
O2 Zn1 O2 118.93(6) 3 2
O2 Zn1 O1W 104.2(8) . 3
O2 Zn1 O1W 103.4(8) 3 3
O2 Zn1 O1W 79.9(5) 2 3
O2 Zn1 O1W 79.9(5) . 2
O2 Zn1 O1W 104.2(8) 3 2
O2 Zn1 O1W 103.4(8) 2 2
O1W Zn1 O1W 27.8(9) 3 2
O2 Zn1 O1W 103.4(8) . .
O2 Zn1 O1W 79.9(5) 3 .
O2 Zn1 O1W 104.2(8) 2 .
O1W Zn1 O1W 27.8(9) 3 .
O1W Zn1 O1W 27.8(9) 2 .
O1 Cu1 N2 93.5(2) . .
O1 Cu1 N1 174.1(2) . .
N2 Cu1 N1 83.4(2) . .
O1 Cu1 Cl1 89.73(15) . .
N2 Cu1 Cl1 170.0(2) . .
N1 Cu1 Cl1 92.51(17) . .
O1 Cu1 Cl1 92.02(17) . 14_445
N2 Cu1 Cl1 88.4(2) . 14_445
N1 Cu1 Cl1 92.92(19) . 14_445
Cl1 Cu1 Cl1 100.93(11) . 14_445
O3 Cu2 O3 94.9(3) . 12
O3 Cu2 O3 85.1(3) . 3
O3 Cu2 O3 180.0(6) 12 3
O3 Cu2 O3 85.1(3) . 2
O3 Cu2 O3 94.9(3) 12 2
O3 Cu2 O3 85.1(3) 3 2
O3 Cu2 O3 94.9(3) . 11
O3 Cu2 O3 85.1(3) 12 11
O3 Cu2 O3 94.9(3) 3 11
O3 Cu2 O3 180.0(4) 2 11
O3 Cu2 O3 180.0(3) . 10
O3 Cu2 O3 85.1(3) 12 10
O3 Cu2 O3 94.9(3) 3 10
O3 Cu2 O3 94.9(3) 2 10
O3 Cu2 O3 85.1(3) 11 10
Cu1 Cl1 Cu1 117.65(7) . 15_455
C13 O1 Cu1 126.9(4) . .
C14 O2 Zn1 119.8(5) . .
C14 O3 Cu2 161.0(7) . .
C1A N1 Cu1 111.0(5) . .
C1 N1 Cu1 108.0(4) . .
C7 N2 C6A 119.7(6) . .
C7 N2 C6 119.6(6) . .
C7 N2 Cu1 126.1(5) . .
C6A N2 Cu1 111.9(5) . .
C6 N2 Cu1 112.1(4) . .
N2 C7 C8 125.2(6) . .
C9 C8 C13 119.9(6) . .
C9 C8 C7 117.3(6) . .
C13 C8 C7 122.8(6) . .
C10 C9 C8 122.3(6) . .
C9 C10 C11 117.9(6) . .
C9 C10 C14 121.6(7) . .
C11 C10 C14 120.5(6) . .
C12 C11 C10 121.1(6) . .
C11 C12 C13 122.4(7) . .
O1 C13 C12 118.4(6) . .
O1 C13 C8 125.3(6) . .
C12 C13 C8 116.3(6) . .
O3 C14 O2 123.8(8) . .
O3 C14 C10 118.5(8) . .
O2 C14 C10 117.8(7) . .
C2 C1 C6 110.3(7) . .
C2 C1 N1 110.9(8) . .
C6 C1 N1 106.0(8) . .
C3 C2 C1 115.3(7) . .
C2 C3 C4 112.2(11) . .
C3 C4 C5 113.3(10) . .
C6 C5 C4 114.9(7) . .
C5 C6 C1 107.9(8) . .
C5 C6 N2 112.7(7) . .
C1 C6 N2 99.4(7) . .
C1A C6A C5A 113.3(10) . .
C1A C6A N2 103.2(10) . .
C5A C6A N2 113.5(10) . .
C4A C3A C2A 110.5(9) . .
N1 C1A C6A 112.3(11) . .
N1 C1A C2A 117.8(10) . .
C6A C1A C2A 110.4(9) . .
C3A C4A C5A 108.2(9) . .
C1A C2A C3A 115.2(7) . .
C6A C5A C4A 115.0(7) . .
O1W O1W O1W 59.997(4) 2 3
O1W O1W Zn1 76.1(4) 2 .
O1W O1W Zn1 76.1(4) 3 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O2 1.917(5) .
Zn1 O2 1.917(5) 3
Zn1 O2 1.917(5) 2
Zn1 O1W 2.125(19) 3
Zn1 O1W 2.125(19) 2
Zn1 O1W 2.125(19) .
Cu1 O1 1.906(4) .
Cu1 N2 1.964(6) .
Cu1 N1 1.996(5) .
Cu1 Cl1 2.293(2) .
Cu1 Cl1 2.877(2) 14_445
Cu2 O3 2.242(5) .
Cu2 O3 2.242(5) 12
Cu2 O3 2.242(5) 3
Cu2 O3 2.242(5) 2
Cu2 O3 2.242(5) 11
Cu2 O3 2.242(5) 10
Cl1 Cu1 2.877(2) 15_455
O1 C13 1.302(8) .
O2 C14 1.254(10) .
O3 C14 1.241(10) .
N1 C1A 1.425(15) .
N1 C1 1.526(14) .
N2 C7 1.279(9) .
N2 C6A 1.534(14) .
N2 C6 1.553(12) .
C7 C8 1.440(9) .
C8 C9 1.396(9) .
C8 C13 1.429(9) .
C9 C10 1.364(9) .
C10 C11 1.409(11) .
C10 C14 1.480(10) .
C11 C12 1.354(11) .
C12 C13 1.407(9) .
C1 C2 1.515(8) .
C1 C6 1.524(9) .
C2 C3 1.484(9) .
C3 C4 1.495(10) .
C4 C5 1.514(9) .
C5 C6 1.510(8) .
C6A C1A 1.498(9) .
C6A C5A 1.514(9) .
C3A C4A 1.513(9) .
C3A C2A 1.528(9) .
C1A C2A 1.499(9) .
C4A C5A 1.519(9) .
O1W O1W 1.02(3) 2
O1W O1W 1.02(3) 3
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C6A N2 C7 C8 -157.0(10)
C6 N2 C7 C8 165.7(8)
Cu1 N2 C7 C8 4.1(13)
N2 C7 C8 C9 179.2(8)
N2 C7 C8 C13 0.6(13)
C13 C8 C9 C10 0.7(11)
C7 C8 C9 C10 -178.0(7)
C8 C9 C10 C11 1.0(11)
C8 C9 C10 C14 -178.6(7)
C9 C10 C11 C12 -1.3(13)
C14 C10 C11 C12 178.3(8)
C10 C11 C12 C13 -0.1(14)
Cu1 O1 C13 C12 -178.9(5)
Cu1 O1 C13 C8 1.1(10)
C11 C12 C13 O1 -178.2(8)
C11 C12 C13 C8 1.8(12)
C9 C8 C13 O1 177.9(7)
C7 C8 C13 O1 -3.4(12)
C9 C8 C13 C12 -2.1(10)
C7 C8 C13 C12 176.5(7)
Cu2 O3 C14 O2 -1(3)
Cu2 O3 C14 C10 180.0(18)
Zn1 O2 C14 O3 3.4(12)
Zn1 O2 C14 C10 -177.2(5)
C9 C10 C14 O3 -172.8(8)
C11 C10 C14 O3 7.5(12)
C9 C10 C14 O2 7.8(11)
C11 C10 C14 O2 -171.9(8)
Cu1 N1 C1 C2 -167.1(6)
Cu1 N1 C1 C6 -47.4(9)
C6 C1 C2 C3 31.5(16)
N1 C1 C2 C3 148.5(12)
C1 C2 C3 C4 27(2)
C2 C3 C4 C5 -54(3)
C3 C4 C5 C6 20(2)
C4 C5 C6 C1 37.7(15)
C4 C5 C6 N2 146.5(13)
C2 C1 C6 C5 -64.4(12)
N1 C1 C6 C5 175.5(7)
C2 C1 C6 N2 178.0(8)
N1 C1 C6 N2 57.8(9)
C7 N2 C6 C5 36.4(11)
Cu1 N2 C6 C5 -159.7(6)
C7 N2 C6 C1 150.4(9)
Cu1 N2 C6 C1 -45.6(9)
C7 N2 C6A C1A -158.5(12)
Cu1 N2 C6A C1A 37.9(14)
C7 N2 C6A C5A -35.4(15)
Cu1 N2 C6A C5A 160.9(8)
Cu1 N1 C1A C6A 34.2(16)
Cu1 N1 C1A C2A 164.1(10)
C5A C6A C1A N1 -169.2(12)
N2 C6A C1A N1 -46.1(17)
C5A C6A C1A C2A 57(2)
N2 C6A C1A C2A -179.7(12)
C2A C3A C4A C5A 63.3(16)
N1 C1A C2A C3A -153.0(12)
C6A C1A C2A C3A -22.2(19)
C4A C3A C2A C1A -37.3(16)
C1A C6A C5A C4A -30.3(18)
N2 C6A C5A C4A -147.6(11)
C3A C4A C5A C6A -29.2(17)
