#------------------------------------------------------------------------------
#$Date: 2017-04-21 05:23:09 +0300 (Fri, 21 Apr 2017) $
#$Revision: 195645 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/27/7042737.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_7042737
loop_
_publ_author_name
'Song, You'
'Yang, Li'
'Li, Jing'
'Pu, Tian-Cheng'
'Kong, Ming'
_publ_section_title
;
 Metal-ion induced ferromagnetic polarization in mixed-spin system
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00753A
_journal_year                    2017
_chemical_formula_sum            'C48 H45 Cl Cu3 O24 Zn'
_chemical_formula_weight         1297.28
_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-2016/6
_audit_update_record
;
2017-03-28 deposited with the CCDC.
2017-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   12.896(8)
_cell_length_b                   12.896(8)
_cell_length_c                   53.12(3)
_cell_measurement_reflns_used    4044
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.024
_cell_measurement_theta_min      1.978
_cell_volume                     7651(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       70
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            22146
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.024
_diffrn_reflns_theta_min         1.978
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.838
_exptl_absorpt_correction_T_max  0.729
_exptl_absorpt_correction_T_min  0.632
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bulk
_exptl_crystal_F_000             3954
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         4044
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0951P)²+0.7590P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1427
_refine_ls_wR_factor_ref         0.1636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2607
_reflns_number_total             4044
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt00753a2.cif
_cod_data_source_block           1
_cod_original_cell_volume        7651(10)
_cod_database_code               7042737
_shelx_shelxl_version_number     2016/6
_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   0.710
_shelx_estimated_absorpt_t_max   0.745
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
Zn1 Zn 0.333333 0.666667 0.51857(2) 0.0444(2) Uani 1 3 d S T P
Cu1 Cu 0.44276(4) 0.61405(4) 0.57114(2) 0.0441(2) Uani 1 1 d . . .
O1 O 0.333333 0.666667 0.58412(8) 0.0432(10) Uani 1 3 d S T P
H1 H 0.333330 0.666668 0.602569 0.052 Uiso 1 3 calc R U P
O2 O 0.6315(3) 0.7698(3) 0.57883(5) 0.0639(9) Uani 1 1 d . . .
O3 O 0.4804(2) 0.7281(3) 0.54223(5) 0.0461(7) Uani 1 1 d . . .
O4 O 0.4430(3) 0.8108(3) 0.49537(6) 0.0646(9) Uani 1 1 d . . .
O5 O 0.5048(3) 0.5281(3) 0.55199(5) 0.0592(8) Uani 1 1 d . . .
O6 O 0.4158(3) 0.5208(3) 0.60039(6) 0.0590(8) Uani 1 1 d . . .
O7 O 0.3587(4) 0.4177(4) 0.64375(6) 0.0801(11) Uani 1 1 d . . .
C1 C 0.7028(6) 0.7949(6) 0.60106(10) 0.092(2) Uani 1 1 d . . .
H1A H 0.652893 0.748397 0.614820 0.138 Uiso 1 1 calc R U .
H1B H 0.739177 0.878536 0.605030 0.138 Uiso 1 1 calc R U .
H1C H 0.764030 0.774611 0.598261 0.138 Uiso 1 1 calc R U .
C2 C 0.6751(4) 0.8455(4) 0.55867(8) 0.0472(9) Uani 1 1 d . . .
C3 C 0.7896(4) 0.9414(4) 0.55683(9) 0.0640(12) Uani 1 1 d . . .
H3 H 0.843696 0.957439 0.569872 0.077 Uiso 1 1 calc R U .
C4 C 0.8248(5) 1.0136(5) 0.53590(11) 0.0737(15) Uani 1 1 d . . .
H4 H 0.902845 1.077299 0.534701 0.088 Uiso 1 1 calc R U .
C5 C 0.7457(5) 0.9922(4) 0.51691(9) 0.0647(13) Uani 1 1 d . . .
H5 H 0.769935 1.042272 0.502919 0.078 Uiso 1 1 calc R U .
C6 C 0.6261(4) 0.8939(4) 0.51824(8) 0.0477(9) Uani 1 1 d . . .
C7 C 0.5906(3) 0.8198(3) 0.53928(7) 0.0418(9) Uani 1 1 d . . .
C8 C 0.5479(5) 0.8836(4) 0.49810(9) 0.0608(12) Uani 1 1 d . . .
H8 H 0.582344 0.940590 0.485411 0.073 Uiso 1 1 calc R U .
C9 C 0.5026(4) 0.4356(5) 0.55973(8) 0.0568(11) Uani 1 1 d . . .
H9 H 0.527328 0.397940 0.548241 0.068 Uiso 1 1 calc R U .
C10 C 0.4677(4) 0.3808(4) 0.58340(9) 0.0554(11) Uani 1 1 d . . .
C11 C 0.4786(6) 0.2784(5) 0.58815(14) 0.093(2) Uani 1 1 d . . .
H11 H 0.502973 0.245487 0.575485 0.112 Uiso 1 1 calc R U .
C12 C 0.4529(8) 0.2293(6) 0.61153(16) 0.121(3) Uani 1 1 d . . .
H12 H 0.461562 0.163129 0.614696 0.145 Uiso 1 1 calc R U .
C13 C 0.4149(6) 0.2730(6) 0.63049(12) 0.099(2) Uani 1 1 d . . .
H13 H 0.400830 0.238040 0.646361 0.119 Uiso 1 1 calc R U .
C14 C 0.3971(5) 0.3681(5) 0.62647(10) 0.0685(14) Uani 1 1 d . . .
C15 C 0.4276(4) 0.4280(4) 0.60245(8) 0.0508(10) Uani 1 1 d . . .
C16 C 0.3214(7) 0.3599(8) 0.66788(11) 0.113(3) Uani 1 1 d . . .
H16A H 0.256067 0.279765 0.665650 0.170 Uiso 1 1 calc R U .
H16B H 0.296101 0.403942 0.678327 0.170 Uiso 1 1 calc R U .
H16C H 0.387169 0.357565 0.675769 0.170 Uiso 1 1 calc R U .
Cl1 Cl 1.000000 1.000000 0.63377(5) 0.0776(6) Uani 1 3 d S T P
O9 O 0.9336(10) 0.8876(6) 0.64233(14) 0.237(5) Uani 1 1 d . . .
O10 O 1.000000 1.000000 0.60640(14) 0.102(2) Uani 1 3 d S T P
O8 O 0.333333 0.666667 0.63528(17) 0.157(4) Uani 1 3 d S T P
H8A H 0.323480 0.708860 0.646227 0.236 Uiso 0.3333 1 d R U P
H8B H 0.315860 0.599400 0.641647 0.236 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 0.0033 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'
Zn Zn 0.2839 1.4301 '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
O3 Zn1 O3 87.10(11) 2_665 3_565
O3 Zn1 O3 87.10(11) 2_665 .
O3 Zn1 O3 87.10(11) 3_565 .
O3 Zn1 O4 98.79(13) 2_665 .
O3 Zn1 O4 170.87(12) 3_565 .
O3 Zn1 O4 86.25(12) . .
O3 Zn1 O4 86.25(12) 2_665 2_665
O3 Zn1 O4 98.79(14) 3_565 2_665
O3 Zn1 O4 170.87(12) . 2_665
O4 Zn1 O4 88.60(14) . 2_665
O3 Zn1 O4 170.87(13) 2_665 3_565
O3 Zn1 O4 86.25(12) 3_565 3_565
O3 Zn1 O4 98.79(13) . 3_565
O4 Zn1 O4 88.60(14) . 3_565
O4 Zn1 O4 88.60(14) 2_665 3_565
O6 Cu1 O5 93.70(13) . .
O6 Cu1 O1 89.75(15) . .
O5 Cu1 O1 161.38(13) . .
O6 Cu1 O3 174.18(14) . .
O5 Cu1 O3 89.98(12) . .
O1 Cu1 O3 88.18(13) . .
O6 Cu1 O2 100.87(13) . .
O5 Cu1 O2 91.91(14) . .
O1 Cu1 O2 105.41(10) . .
O3 Cu1 O2 74.47(11) . .
Cu1 O1 Cu1 108.43(12) 2_665 3_565
Cu1 O1 Cu1 108.43(12) 2_665 .
Cu1 O1 Cu1 108.43(13) 3_565 .
Cu1 O1 H1 110.5 2_665 .
Cu1 O1 H1 110.5 3_565 .
Cu1 O1 H1 110.5 . .
C2 O2 C1 119.8(4) . .
C2 O2 Cu1 111.3(2) . .
C1 O2 Cu1 128.8(3) . .
C7 O3 Cu1 120.1(2) . .
C7 O3 Zn1 129.5(2) . .
Cu1 O3 Zn1 110.05(13) . .
C8 O4 Zn1 128.2(3) . .
C9 O5 Cu1 123.5(3) . .
C15 O6 Cu1 126.4(3) . .
C14 O7 C16 118.0(5) . .
O2 C1 H1A 109.5 . .
O2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
O2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
O2 C2 C3 124.8(4) . .
O2 C2 C7 114.2(4) . .
C3 C2 C7 120.9(4) . .
C4 C3 C2 120.6(5) . .
C4 C3 H3 119.7 . .
C2 C3 H3 119.7 . .
C5 C4 C3 120.2(5) . .
C5 C4 H4 119.9 . .
C3 C4 H4 119.9 . .
C4 C5 C6 120.7(4) . .
C4 C5 H5 119.6 . .
C6 C5 H5 119.6 . .
C7 C6 C5 119.2(4) . .
C7 C6 C8 124.2(4) . .
C5 C6 C8 116.4(4) . .
O3 C7 C6 123.0(4) . .
O3 C7 C2 118.6(3) . .
C6 C7 C2 118.3(4) . .
O4 C8 C6 128.7(4) . .
O4 C8 H8 115.7 . .
C6 C8 H8 115.7 . .
O5 C9 C10 128.7(4) . .
O5 C9 H9 115.6 . .
C10 C9 H9 115.6 . .
C9 C10 C15 121.5(4) . .
C9 C10 C11 118.2(5) . .
C15 C10 C11 120.2(5) . .
C12 C11 C10 118.8(6) . .
C12 C11 H11 120.6 . .
C10 C11 H11 120.6 . .
C11 C12 C13 122.7(6) . .
C11 C12 H12 118.7 . .
C13 C12 H12 118.7 . .
C12 C13 C14 120.7(5) . .
C12 C13 H13 119.6 . .
C14 C13 H13 119.6 . .
O7 C14 C13 125.7(5) . .
O7 C14 C15 114.6(4) . .
C13 C14 C15 119.6(5) . .
O6 C15 C10 125.6(4) . .
O6 C15 C14 116.5(4) . .
C10 C15 C14 117.9(4) . .
O7 C16 H16A 109.5 . .
O7 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
O7 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
O9 Cl1 O9 109.1(4) . 3_675
O9 Cl1 O9 109.1(4) . 2_765
O9 Cl1 O9 109.1(4) 3_675 2_765
O9 Cl1 O10 109.8(4) . .
O9 Cl1 O10 109.8(4) 3_675 .
O9 Cl1 O10 109.8(4) 2_765 .
H8A O8 H8B 109.5 . .
H8A O8 H8A 78.1 . 2_665
H8B O8 H8A 35.1 . 2_665
H8A O8 H8A 78.1 . 3_565
H8B O8 H8A 70.5 . 3_565
H8A O8 H8A 78.1 2_665 3_565
H8A O8 H8B 70.5 . 2_665
H8B O8 H8B 105.2 . 2_665
H8A O8 H8B 109.5 2_665 2_665
H8A O8 H8B 35.1 3_565 2_665
H8A O8 H8B 35.1 . 3_565
H8B O8 H8B 105.2 . 3_565
H8A O8 H8B 70.5 2_665 3_565
H8A O8 H8B 109.5 3_565 3_565
H8B O8 H8B 105.2 2_665 3_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O3 2.074(3) 2_665
Zn1 O3 2.074(3) 3_565
Zn1 O3 2.074(3) .
Zn1 O4 2.084(3) .
Zn1 O4 2.084(3) 2_665
Zn1 O4 2.084(3) 3_565
Cu1 O6 1.888(3) .
Cu1 O5 1.947(3) .
Cu1 O1 1.9710(19) .
Cu1 O3 2.011(3) .
Cu1 O2 2.288(3) .
O1 H1 0.9800 .
O2 C2 1.366(5) .
O2 C1 1.431(6) .
O3 C7 1.326(5) .
O4 C8 1.210(6) .
O5 C9 1.249(6) .
O6 C15 1.284(5) .
O7 C14 1.346(7) .
O7 C16 1.439(6) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 C3 1.376(7) .
C2 C7 1.413(6) .
C3 C4 1.374(7) .
C3 H3 0.9300 .
C4 C5 1.361(7) .
C4 H4 0.9300 .
C5 C6 1.427(7) .
C5 H5 0.9300 .
C6 C7 1.391(5) .
C6 C8 1.430(6) .
C8 H8 0.9300 .
C9 C10 1.402(6) .
C9 H9 0.9300 .
C10 C15 1.406(6) .
C10 C11 1.419(7) .
C11 C12 1.357(10) .
C11 H11 0.9300 .
C12 C13 1.359(9) .
C12 H12 0.9300 .
C13 C14 1.374(8) .
C13 H13 0.9300 .
C14 C15 1.440(6) .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
Cl1 O9 1.342(6) .
Cl1 O9 1.342(6) 3_675
Cl1 O9 1.342(6) 2_765
Cl1 O10 1.454(8) .
O8 H8A 0.8484 .
O8 H8B 0.8499 .
O8 H8A 0.8485 2_665
O8 H8A 0.8484 3_565
O8 H8B 0.8498 2_665
O8 H8B 0.8498 3_565
