#------------------------------------------------------------------------------
#$Date: 2016-03-26 17:08:36 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180413 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/82/7208239.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_7208239
loop_
_publ_author_name
'Wang, Nan'
'Ma, Jian-Gong'
'Shi, Wei'
'Cheng, Peng'
_publ_section_title
;
 Two novel Cd(ii) complexes with unprecedented four- and six-fold
 interpenetration
;
_journal_issue                   16
_journal_name_full               CrystEngComm
_journal_page_first              5198
_journal_paper_doi               10.1039/c2ce25282a
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C54 H56 Cd Cl2 N18 O12'
_chemical_formula_weight         1332.47
_chemical_name_systematic
;
?
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   10.6908(3)
_cell_length_b                   10.6908(3)
_cell_length_c                   92.650(2)
_cell_measurement_reflns_used    5132
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1558
_cell_measurement_theta_min      2.4542
_cell_volume                     9170.6(4)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0169
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       109
_diffrn_reflns_limit_l_min       -109
_diffrn_reflns_number            10566
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    0.519
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90410
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             4104
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.961
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         1809
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1005P)²+20.7718P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1610
_reflns_number_gt                1531
_reflns_number_total             1809
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25282a.txt
_cod_data_source_block           p110410h
_cod_original_sg_symbol_H-M      R-3c
_cod_database_code               7208239
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'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-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'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+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-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+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-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+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cd1 Cd 0.0000 0.0000 1.0000 0.0430(3) Uani 1 6 d S .
C1 C 0.2284(4) 0.2283(5) 0.97611(4) 0.0551(10) Uani 1 1 d . .
H1 H 0.1734 0.2732 0.9752 0.066 Uiso 1 1 calc R .
C2 C 0.3846(6) 0.1673(6) 0.97265(6) 0.0770(15) Uani 1 1 d . .
H2 H 0.4615 0.1606 0.9688 0.092 Uiso 1 1 calc R .
C3B C 0.4009(15) 0.3686(17) 0.9566(2) 0.046(3) Uani 0.62(3) 1 d PDU 2
C4B C 0.4344(17) 0.506(2) 0.9587(3) 0.066(4) Uani 0.62(3) 1 d PDU 2
H4B H 0.4207 0.5347 0.9678 0.079 Uiso 0.62(3) 1 calc PR 2
C5B C 0.4879(15) 0.6027(13) 0.94784(15) 0.074(3) Uani 0.62(3) 1 d PDU 2
H5B H 0.5103 0.6972 0.9497 0.089 Uiso 0.62(3) 1 calc PR 2
C6B C 0.5106(15) 0.5694(10) 0.93437(12) 0.073(3) Uani 0.62(3) 1 d PDU 2
C7B C 0.4730(16) 0.4229(13) 0.93168(13) 0.078(3) Uani 0.62(3) 1 d PDU 2
H7B H 0.4873 0.3960 0.9226 0.094 Uiso 0.62(3) 1 calc PR 2
C8B C 0.4143(16) 0.3191(14) 0.94277(15) 0.067(3) Uani 0.62(3) 1 d PDU 2
H8B H 0.3858 0.2226 0.9411 0.080 Uiso 0.62(3) 1 calc PR 2
C9B C 0.5637(16) 0.6856(12) 0.92276(10) 0.111(5) Uani 0.601(18) 1 d PDU 2
H9BA H 0.5176 0.7428 0.9244 0.134 Uiso 0.601(18) 1 calc PR 2
H9BB H 0.6666 0.7491 0.9242 0.134 Uiso 0.601(18) 1 calc PR 2
Cl1 Cl 1.0000 1.0000 0.94398(2) 0.0591(5) Uani 1 3 d S .
N1 N 0.2025(4) 0.1269(4) 0.98525(3) 0.0537(9) Uani 1 1 d . .
N2 N 0.3037(5) 0.0869(5) 0.98310(5) 0.0760(12) Uani 1 1 d . .
N3 N 0.3454(3) 0.2605(3) 0.96803(3) 0.0511(8) Uani 1 1 d . .
O1 O 0.8655(4) 0.8868(4) 0.94930(4) 0.0937(12) Uani 1 1 d . .
O2 O 1.0000 1.0000 0.92881(8) 0.125(4) Uani 1 3 d S .
C9 C 0.6332(14) 0.6439(15) 0.92088(12) 0.071(5) Uani 0.399(18) 1 d PU 1
H9A H 0.6603 0.7299 0.9266 0.085 Uiso 0.399(18) 1 calc PR 1
H9B H 0.7184 0.6338 0.9214 0.085 Uiso 0.399(18) 1 calc PR 1
C6A C 0.5531(17) 0.5370(19) 0.93339(16) 0.060(5) Uani 0.38(3) 1 d PDU 1
C7A C 0.516(2) 0.400(2) 0.9326(2) 0.070(5) Uani 0.38(3) 1 d PDU 1
H7A H 0.5321 0.3632 0.9241 0.084 Uiso 0.38(3) 1 calc PR 1
C8A C 0.452(2) 0.311(2) 0.9445(2) 0.063(5) Uani 0.38(3) 1 d PDU 1
H8A H 0.4339 0.2163 0.9439 0.075 Uiso 0.38(3) 1 calc PR 1
C3A C 0.415(3) 0.348(3) 0.9561(4) 0.045(6) Uani 0.38(3) 1 d PDU 1
C5A C 0.527(2) 0.592(2) 0.9458(2) 0.065(5) Uani 0.38(3) 1 d PDU 1
H5A H 0.5561 0.6895 0.9465 0.078 Uiso 0.38(3) 1 calc PR 1
C4A C 0.454(3) 0.495(4) 0.9577(4) 0.059(7) Uani 0.38(3) 1 d PDU 1
H4A H 0.4335 0.5282 0.9661 0.071 Uiso 0.38(3) 1 calc PR 1
O3 O 0.4345(18) 0.9302(18) 0.99825(18) 0.171(5) Uani 0.50 1 d PU .
O4 O 0.6667 0.3333 0.0051(4) 0.258(19) Uani 0.50 3 d SP .
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'
Cd Cd -0.8075 1.2024 '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'
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'
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
N1 Cd1 N1 89.24(12) 21_557 19_557
N1 Cd1 N1 89.24(12) 21_557 20_557
N1 Cd1 N1 89.24(12) 19_557 20_557
N1 Cd1 N1 90.76(12) 21_557 .
N1 Cd1 N1 180.00(12) 19_557 .
N1 Cd1 N1 90.76(12) 20_557 .
N1 Cd1 N1 180.000(4) 21_557 3
N1 Cd1 N1 90.76(13) 19_557 3
N1 Cd1 N1 90.76(12) 20_557 3
N1 Cd1 N1 89.24(12) . 3
N1 Cd1 N1 90.76(12) 21_557 2
N1 Cd1 N1 90.76(12) 19_557 2
N1 Cd1 N1 180.00(12) 20_557 2
N1 Cd1 N1 89.24(12) . 2
N1 Cd1 N1 89.24(12) 3 2
N1 C1 N3 111.2(4) . .
N1 C1 H1 124.4 . .
N3 C1 H1 124.4 . .
N2 C2 N3 112.4(4) . .
N2 C2 H2 123.8 . .
N3 C2 H2 123.8 . .
C4B C3B C8B 121.6(18) . .
C4B C3B N3 122.5(17) . .
C8B C3B N3 116.0(12) . .
C3B C4B C5B 120(2) . .
C3B C4B H4B 119.9 . .
C5B C4B H4B 119.9 . .
C4B C5B C6B 123.4(13) . .
C4B C5B H5B 118.3 . .
C6B C5B H5B 118.3 . .
C5B C6B C7B 117.4(9) . .
C5B C6B C9B 118.7(10) . .
C7B C6B C9B 123.8(11) . .
C8B C7B C6B 120.4(11) . .
C8B C7B H7B 119.8 . .
C6B C7B H7B 119.8 . .
C7B C8B C3B 116.8(12) . .
C7B C8B H8B 121.6 . .
C3B C8B H8B 121.6 . .
C9B C9B C6B 117.7(14) 10_566 .
C9B C9B H9BA 107.9 10_566 .
C6B C9B H9BA 107.9 . .
C9B C9B H9BB 107.9 10_566 .
C6B C9B H9BB 107.9 . .
H9BA C9B H9BB 107.2 . .
O2 Cl1 O1 110.19(19) . 3_675
O2 Cl1 O1 110.19(19) . 2_765
O1 Cl1 O1 108.7(2) 3_675 2_765
O2 Cl1 O1 110.19(19) . .
O1 Cl1 O1 108.75(19) 3_675 .
O1 Cl1 O1 108.75(19) 2_765 .
C1 N1 N2 107.2(3) . .
C1 N1 Cd1 128.2(3) . .
N2 N1 Cd1 123.7(3) . .
C2 N2 N1 105.9(4) . .
C2 N3 C1 103.3(3) . .
C2 N3 C3A 119.5(11) . .
C1 N3 C3A 136.6(11) . .
C2 N3 C3B 132.2(8) . .
C1 N3 C3B 124.4(7) . .
C3A N3 C3B 12.9(15) . .
C9 C9 C6A 164(2) 10_566 .
C9 C9 H9A 95.0 10_566 .
C6A C9 H9A 95.0 . .
C9 C9 H9B 95.0 10_566 .
C6A C9 H9B 95.0 . .
H9A C9 H9B 103.2 . .
C7A C6A C5A 120.6(16) . .
C7A C6A C9 121.8(17) . .
C5A C6A C9 117.5(16) . .
C6A C7A C8A 119.3(19) . .
C6A C7A H7A 120.4 . .
C8A C7A H7A 120.4 . .
C3A C8A C7A 125(2) . .
C3A C8A H8A 117.5 . .
C7A C8A H8A 117.5 . .
C8A C3A N3 127(2) . .
C8A C3A C4A 118(3) . .
N3 C3A C4A 115(3) . .
C6A C5A C4A 119(2) . .
C6A C5A H5A 120.6 . .
C4A C5A H5A 120.6 . .
C3A C4A C5A 118(3) . .
C3A C4A H4A 121.0 . .
C5A C4A H4A 121.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 N1 2.336(3) 21_557
Cd1 N1 2.336(4) 19_557
Cd1 N1 2.336(3) 20_557
Cd1 N1 2.336(4) .
Cd1 N1 2.336(3) 3
Cd1 N1 2.336(3) 2
C1 N1 1.292(5) .
C1 N3 1.346(5) .
C1 H1 0.9300 .
C2 N2 1.296(6) .
C2 N3 1.330(6) .
C2 H2 0.9300 .
C3B C4B 1.34(3) .
C3B C8B 1.42(2) .
C3B N3 1.460(19) .
C4B C5B 1.35(3) .
C4B H4B 0.9300 .
C5B C6B 1.353(18) .
C5B H5B 0.9300 .
C6B C7B 1.431(17) .
C6B C9B 1.522(9) .
C7B C8B 1.409(17) .
C7B H7B 0.9300 .
C8B H8B 0.9300 .
C9B C9B 1.182(19) 10_566
C9B H9BA 0.9700 .
C9B H9BB 0.9700 .
Cl1 O2 1.406(7) .
Cl1 O1 1.426(4) 3_675
Cl1 O1 1.426(4) 2_765
Cl1 O1 1.426(4) .
N1 N2 1.362(5) .
N3 C3A 1.40(4) .
C9 C9 0.887(19) 10_566
C9 C6A 1.551(17) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C6A C7A 1.31(3) .
C6A C5A 1.38(3) .
C7A C8A 1.40(3) .
C7A H7A 0.9300 .
C8A C3A 1.27(4) .
C8A H8A 0.9300 .
C3A C4A 1.42(4) .
C5A C4A 1.45(4) .
C5A H5A 0.9300 .
C4A H4A 0.9300 .
O3 O3 1.48(4) 19_677
