#------------------------------------------------------------------------------
#$Date: 2018-12-19 01:02:42 +0200 (Wed, 19 Dec 2018) $
#$Revision: 212642 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/27/7122751.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_7122751
loop_
_publ_author_name
'Hayashi, Daiki'
'Yoshinari, Nobuto'
'Konno, Takumi'
_publ_section_title
;
 Conversion of 12-Membered D3- and L3-CoIII3CdII3 Metallorings into a
 24-Membered D3L3-CoIII6CdII6 Metalloring
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC09121H
_journal_year                    2018
_chemical_formula_moiety         'C72 H120 Cd6 Cl6 Co6 N12 O30 S12, 12(O)'
_chemical_formula_sum            'C72 H156 Cd6 Cl6 Co6 N12 O42 S12'
_chemical_formula_weight         3487.48
_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   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-11-16 deposited with the CCDC.
2018-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   34.066(12)
_cell_length_b                   34.066(12)
_cell_length_c                   8.8283(16)
_cell_measurement_reflns_used    10157
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.17
_cell_volume                     8873(5)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'Mercury 3.10'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku FR-E SuperBright'
_diffrn_measurement_method       'Rigaku R-AXIS VII'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            23165
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         3.164
_exptl_absorpt_coefficient_mu    2.303
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             5256
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.598
_refine_diff_density_min         -1.428
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0462
_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)+(0.0422P)²+55.5021P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4098
_reflns_number_total             4520
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cc09121h2.cif
_cod_data_source_block           D3L3-2Cl
_cod_original_cell_volume        8873(6)
_cod_database_code               7122751
_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   0.855
_shelx_estimated_absorpt_t_max   0.934
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
Cd1 Cd 0.22220(2) 0.10562(2) 0.42686(4) 0.03582(12) Uani 1 1 d . .
Co1 Co 0.17858(2) -0.01198(2) 0.38296(7) 0.03235(15) Uani 1 1 d . .
Cl1 Cl 0.25846(4) 0.11383(4) 0.16316(15) 0.0480(3) Uani 1 1 d . .
S1 S 0.14638(3) 0.02919(3) 0.44908(13) 0.0336(2) Uani 1 1 d . .
S2 S 0.18011(3) -0.04021(3) 0.61045(14) 0.0359(2) Uani 1 1 d . .
O1 O 0.27719(11) 0.12761(12) 0.6020(4) 0.0489(8) Uani 1 1 d . .
O2 O 0.12175(9) -0.06430(9) 0.3337(3) 0.0345(6) Uani 1 1 d . .
O3 O 0.06518(10) -0.08778(10) 0.1649(4) 0.0420(7) Uani 1 1 d . .
O4 O 0.23742(10) 0.03906(10) 0.4217(4) 0.0420(8) Uani 1 1 d . .
O5 O 0.30935(12) 0.05554(12) 0.4502(7) 0.0884(17) Uani 1 1 d . .
N1 N 0.17446(12) 0.00557(11) 0.1754(4) 0.0346(8) Uani 1 1 d . .
H1 H 0.1938 0.0391 0.1614 0.041 Uiso 1 1 calc R U
N2 N 0.21380(12) -0.03871(12) 0.3055(5) 0.0415(9) Uani 1 1 d . .
H2 H 0.1954 -0.0726 0.3028 0.050 Uiso 1 1 calc R U
C1 C 0.11460(14) 0.02127(14) 0.2689(5) 0.0342(9) Uani 1 1 d . .
C2 C 0.12550(14) -0.00889(14) 0.1641(5) 0.0347(9) Uani 1 1 d . .
H2A H 0.1170 -0.0072 0.0568 0.042 Uiso 1 1 calc R U
C3 C 0.10071(14) -0.05795(14) 0.2203(5) 0.0360(9) Uani 1 1 d . .
C4 C 0.06370(14) -0.00299(16) 0.3044(6) 0.0409(10) Uani 1 1 d . .
H4 H 0.0546 -0.0323 0.3518 0.061 Uiso 1 1 calc R U
H4A H 0.0574 0.0156 0.3737 0.061 Uiso 1 1 calc R U
H4B H 0.0466 -0.0078 0.2103 0.061 Uiso 1 1 calc R U
C5 C 0.12831(16) 0.06681(15) 0.1953(6) 0.0412(10) Uani 1 1 d . .
H5 H 0.1608 0.0826 0.1722 0.062 Uiso 1 1 calc R U
H5A H 0.1111 0.0619 0.1014 0.062 Uiso 1 1 calc R U
H5B H 0.1218 0.0853 0.2649 0.062 Uiso 1 1 calc R U
C6 C 0.23164(14) -0.04532(14) 0.5759(6) 0.0407(11) Uani 1 1 d . .
C7 C 0.25108(14) -0.02236(15) 0.4207(6) 0.0447(12) Uani 1 1 d . .
H7 H 0.2754 -0.0286 0.3862 0.054 Uiso 1 1 calc R U
C8 C 0.26921(16) 0.02839(17) 0.4324(7) 0.0532(14) Uani 1 1 d . .
C9 C 0.26534(17) -0.02005(18) 0.7044(7) 0.0559(14) Uani 1 1 d . .
H9 H 0.2722 0.0115 0.7070 0.084 Uiso 1 1 calc R U
H9A H 0.2520 -0.0347 0.8013 0.084 Uiso 1 1 calc R U
H9B H 0.2933 -0.0208 0.6869 0.084 Uiso 1 1 calc R U
C10 C 0.22150(16) -0.09433(15) 0.5739(7) 0.0502(13) Uani 1 1 d . .
H10 H 0.2000 -0.1109 0.4923 0.075 Uiso 1 1 calc R U
H10A H 0.2497 -0.0948 0.5568 0.075 Uiso 1 1 calc R U
H10B H 0.2083 -0.1087 0.6712 0.075 Uiso 1 1 calc R U
C11 C 0.18951(17) -0.01958(16) 0.0727(6) 0.0446(11) Uani 1 1 d . .
H11 H 0.1988 -0.0044 -0.0271 0.054 Uiso 1 1 calc R U
H11A H 0.1646 -0.0511 0.0572 0.054 Uiso 1 1 calc R U
C12 C 0.22943(18) -0.01919(19) 0.1513(6) 0.0529(13) Uani 1 1 d . .
H12 H 0.2394 -0.0376 0.0935 0.064 Uiso 1 1 calc R U
H12A H 0.2552 0.0122 0.1588 0.064 Uiso 1 1 calc R U
O6 O 0.45696(14) -0.02090(14) 0.7781(5) 0.0698(11) Uani 1 1 d . .
O7 O 0.49926(11) 0.09587(12) 1.1651(4) 0.0511(8) 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
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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 Cd1 O4 78.70(12) . .
O1 Cd1 Cl1 108.06(10) . .
O4 Cd1 Cl1 77.47(8) . .
O1 Cd1 S2 100.68(9) . 12_556
O4 Cd1 S2 167.88(8) . 12_556
Cl1 Cd1 S2 91.37(4) . 12_556
O1 Cd1 S1 121.77(9) . .
O4 Cd1 S1 69.82(7) . .
Cl1 Cd1 S1 110.98(4) . .
S2 Cd1 S1 119.44(3) 12_556 .
O1 Cd1 O2 77.15(11) . 12_556
O4 Cd1 O2 121.30(10) . 12_556
Cl1 Cd1 O2 161.20(7) . 12_556
S2 Cd1 O2 69.83(7) 12_556 12_556
S1 Cd1 O2 79.32(7) . 12_556
O2 Co1 O4 175.98(14) . .
O2 Co1 N1 82.99(14) . .
O4 Co1 N1 95.31(15) . .
O2 Co1 N2 93.29(14) . .
O4 Co1 N2 83.01(15) . .
N1 Co1 N2 88.25(16) . .
O2 Co1 S2 91.93(10) . .
O4 Co1 S2 89.49(11) . .
N1 Co1 S2 173.39(11) . .
N2 Co1 S2 87.82(13) . .
O2 Co1 S1 93.32(9) . .
O4 Co1 S1 90.16(10) . .
N1 Co1 S1 85.43(11) . .
N2 Co1 S1 170.24(12) . .
S2 Co1 S1 99.12(5) . .
C1 S1 Co1 96.75(14) . .
C1 S1 Cd1 107.12(14) . .
Co1 S1 Cd1 93.14(4) . .
C6 S2 Co1 96.77(16) . .
C6 S2 Cd1 112.26(14) . 11_556
Co1 S2 Cd1 95.50(4) . 11_556
C3 O2 Co1 113.7(3) . .
C3 O2 Cd1 141.0(3) . 11_556
Co1 O2 Cd1 102.65(12) . 11_556
C8 O4 Co1 113.4(3) . .
C8 O4 Cd1 143.7(3) . .
Co1 O4 Cd1 102.89(12) . .
C2 N1 C11 114.6(3) . .
C2 N1 Co1 101.7(3) . .
C11 N1 Co1 107.1(3) . .
C2 N1 H1 111.0 . .
C11 N1 H1 111.0 . .
Co1 N1 H1 111.0 . .
C12 N2 C7 113.9(4) . .
C12 N2 Co1 106.1(3) . .
C7 N2 Co1 101.1(3) . .
C12 N2 H2 111.7 . .
C7 N2 H2 111.7 . .
Co1 N2 H2 111.7 . .
C5 C1 C4 108.9(3) . .
C5 C1 C2 111.4(4) . .
C4 C1 C2 110.1(3) . .
C5 C1 S1 110.9(3) . .
C4 C1 S1 108.8(3) . .
C2 C1 S1 106.8(3) . .
N1 C2 C3 104.8(3) . .
N1 C2 C1 109.8(3) . .
C3 C2 C1 110.1(4) . .
N1 C2 H2A 110.7 . .
C3 C2 H2A 110.7 . .
C1 C2 H2A 110.7 . .
O3 C3 O2 124.2(4) . .
O3 C3 C2 123.5(4) . .
O2 C3 C2 112.3(4) . .
C1 C4 H4 109.5 . .
C1 C4 H4A 109.5 . .
H4 C4 H4A 109.5 . .
C1 C4 H4B 109.5 . .
H4 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C1 C5 H5 109.5 . .
C1 C5 H5A 109.5 . .
H5 C5 H5A 109.5 . .
C1 C5 H5B 109.5 . .
H5 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C10 C6 C9 108.6(4) . .
C10 C6 C7 110.3(4) . .
C9 C6 C7 111.0(4) . .
C10 C6 S2 113.2(3) . .
C9 C6 S2 107.5(3) . .
C7 C6 S2 106.3(3) . .
N2 C7 C8 104.8(4) . .
N2 C7 C6 110.0(3) . .
C8 C7 C6 110.0(4) . .
N2 C7 H7 110.6 . .
C8 C7 H7 110.6 . .
C6 C7 H7 110.6 . .
O5 C8 O4 124.7(5) . .
O5 C8 C7 122.3(4) . .
O4 C8 C7 112.9(4) . .
C6 C9 H9 109.5 . .
C6 C9 H9A 109.5 . .
H9 C9 H9A 109.5 . .
C6 C9 H9B 109.5 . .
H9 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C6 C10 H10 109.5 . .
C6 C10 H10A 109.5 . .
H10 C10 H10A 109.5 . .
C6 C10 H10B 109.5 . .
H10 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
N1 C11 C12 106.1(4) . .
N1 C11 H11 110.5 . .
C12 C11 H11 110.5 . .
N1 C11 H11A 110.5 . .
C12 C11 H11A 110.5 . .
H11 C11 H11A 108.7 . .
N2 C12 C11 107.1(4) . .
N2 C12 H12 110.3 . .
C11 C12 H12 110.3 . .
N2 C12 H12A 110.3 . .
C11 C12 H12A 110.3 . .
H12 C12 H12A 108.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 O1 2.249(3) .
Cd1 O4 2.567(3) .
Cd1 Cl1 2.5841(13) .
Cd1 S2 2.5913(14) 12_556
Cd1 S1 2.6009(14) .
Cd1 O2 2.639(3) 12_556
Co1 O2 1.914(3) .
Co1 O4 1.916(3) .
Co1 N1 1.954(4) .
Co1 N2 1.956(4) .
Co1 S2 2.2386(14) .
Co1 S1 2.2472(13) .
S1 C1 1.866(4) .
S2 C6 1.874(4) .
S2 Cd1 2.5912(14) 11_556
O2 C3 1.311(5) .
O2 Cd1 2.639(3) 11_556
O3 C3 1.227(5) .
O4 C8 1.307(5) .
O5 C8 1.219(6) .
N1 C2 1.488(5) .
N1 C11 1.503(6) .
N1 H1 1.0000 .
N2 C12 1.492(6) .
N2 C7 1.500(6) .
N2 H2 1.0000 .
C1 C5 1.524(6) .
C1 C4 1.534(6) .
C1 C2 1.560(6) .
C2 C3 1.530(6) .
C2 H2A 1.0000 .
C4 H4 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C5 H5 0.9800 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C6 C10 1.526(6) .
C6 C9 1.535(7) .
C6 C7 1.552(7) .
C7 C8 1.521(7) .
C7 H7 1.0000 .
C9 H9 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C10 H10 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C11 C12 1.521(7) .
C11 H11 0.9900 .
C11 H11A 0.9900 .
C12 H12 0.9900 .
C12 H12A 0.9900 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 Cl1 1.00 2.39 3.354(4) 160.7 .
N2 H2 O6 1.00 2.35 3.093(6) 130.1 6_554
C10 H10 O1 0.98 2.29 3.188(6) 151.3 11_556
C11 H11 O7 0.99 2.53 3.396(6) 146.5 8_543
C12 H12 O5 0.99 2.38 3.228(6) 143.2 8_544
C12 H12 O6 0.99 2.56 3.126(7) 116.5 6_554
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
_geom_torsion_site_symmetry_1
Co1 S1 C1 C5 -121.6(3) .
Cd1 S1 C1 C5 -26.2(3) .
Co1 S1 C1 C4 118.7(3) .
Cd1 S1 C1 C4 -145.9(3) .
Co1 S1 C1 C2 -0.1(3) .
Cd1 S1 C1 C2 95.3(3) .
C11 N1 C2 C3 64.8(5) .
Co1 N1 C2 C3 -50.3(3) .
C11 N1 C2 C1 -176.9(4) .
Co1 N1 C2 C1 67.9(3) .
C5 C1 C2 N1 79.9(4) .
C4 C1 C2 N1 -159.2(4) .
S1 C1 C2 N1 -41.3(4) .
C5 C1 C2 C3 -165.3(4) .
C4 C1 C2 C3 -44.4(5) .
S1 C1 C2 C3 73.6(4) .
Co1 O2 C3 O3 175.6(4) .
Cd1 O2 C3 O3 -27.4(7) 11_556
Co1 O2 C3 C2 -4.4(4) .
Cd1 O2 C3 C2 152.6(3) 11_556
N1 C2 C3 O3 -142.4(4) .
C1 C2 C3 O3 99.6(5) .
N1 C2 C3 O2 37.6(5) .
C1 C2 C3 O2 -80.4(4) .
Co1 S2 C6 C10 -114.0(4) .
Cd1 S2 C6 C10 -15.2(4) 11_556
Co1 S2 C6 C9 126.1(3) .
Cd1 S2 C6 C9 -135.1(3) 11_556
Co1 S2 C6 C7 7.2(3) .
Cd1 S2 C6 C7 106.0(3) 11_556
C12 N2 C7 C8 63.1(5) .
Co1 N2 C7 C8 -50.2(4) .
C12 N2 C7 C6 -178.7(4) .
Co1 N2 C7 C6 68.0(4) .
C10 C6 C7 N2 75.6(4) .
C9 C6 C7 N2 -164.0(4) .
S2 C6 C7 N2 -47.5(4) .
C10 C6 C7 C8 -169.5(4) .
C9 C6 C7 C8 -49.1(5) .
S2 C6 C7 C8 67.5(4) .
Co1 O4 C8 O5 176.7(6) .
Cd1 O4 C8 O5 -1.2(11) .
Co1 O4 C8 C7 -3.5(6) .
Cd1 O4 C8 C7 178.6(4) .
N2 C7 C8 O5 -143.1(6) .
C6 C7 C8 O5 98.7(7) .
N2 C7 C8 O4 37.1(6) .
C6 C7 C8 O4 -81.1(5) .
C2 N1 C11 C12 -151.5(4) .
Co1 N1 C11 C12 -39.6(4) .
C7 N2 C12 C11 -153.3(4) .
Co1 N2 C12 C11 -43.0(4) .
N1 C11 C12 N2 55.1(5) .
