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#$Date: 2016-03-26 20:57:10 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180457 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/26/7212651.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_7212651
loop_
_publ_author_name
'Huang, Yong-Qing'
'Shen, Zhong-Liang'
'Zhou, Xia-Ying'
'Okamura, Taka-aki'
'Su, Zhi'
'Fan, Jian'
'Sun, Wei-Yin'
'Yu, Jin-Quan'
'Ueyama, Norikazu'
_publ_section_title
;
 Metal--organic frameworks with oxazoline-containing tripodal ligand:
 structure changes via reaction medium and metal-to-ligand ratio
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              4328
_journal_paper_doi               10.1039/c002874f
_journal_volume                  12
_journal_year                    2010
_chemical_formula_sum            'C36 H39 Cl3 Cu3 N9 O18'
_chemical_formula_weight         1182.73
_chemical_name_systematic
;
[Cu3(OX1)2(MeCN)3](ClO4)3
;
_space_group_IT_number           161
_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                   23.752(2)
_cell_length_b                   23.752
_cell_length_c                   14.2281(12)
_cell_measurement_reflns_used    1771
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.39
_cell_measurement_theta_min      2.97
_cell_volume                     6951.5(8)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_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  0.0980
_diffrn_reflns_av_sigmaI/netI    0.1231
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12129
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    1.620
_exptl_absorpt_correction_T_max  0.9090
_exptl_absorpt_correction_T_min  0.5855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Bruker, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         2856
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.891
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0551
_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)+(0.0039P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.1034
_reflns_number_gt                1628
_reflns_number_total             2856
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c002874f.txt
_cod_data_source_block           2
_cod_original_cell_volume        6951.3(8)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               7212651
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, 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'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+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'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
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
Cu1 Cu 0.51958(4) 0.15322(4) 0.99726(7) 0.0563(3) Uani 1 1 d .
Cl1 Cl 0.54618(12) 0.04249(12) 1.16768(17) 0.0691(6) Uani 1 1 d .
C1 C 0.7152(3) 0.3180(3) 0.8762(4) 0.0396(16) Uani 1 1 d .
H1A H 0.7481 0.3075 0.8761 0.048 Uiso 1 1 calc R
C2 C 0.6510(3) 0.2688(3) 0.8763(5) 0.0397(17) Uani 1 1 d .
C3 C 0.6354(4) 0.2008(4) 0.8803(5) 0.0480(19) Uani 1 1 d .
C4 C 0.6512(5) 0.1184(4) 0.8430(8) 0.088(3) Uani 1 1 d .
H4A H 0.6842 0.1109 0.8707 0.106 Uiso 1 1 calc R
H4B H 0.6380 0.0960 0.7831 0.106 Uiso 1 1 calc R
C5 C 0.5934(4) 0.0956(4) 0.9082(6) 0.064(2) Uani 1 1 d .
H5A H 0.5541 0.0617 0.8790 0.076 Uiso 1 1 calc R
H5B H 0.6006 0.0794 0.9668 0.076 Uiso 1 1 calc R
C6 C 0.6379(3) 0.2672(3) 1.1260(4) 0.0366(15) Uani 1 1 d .
H6A H 0.6185 0.2221 1.1281 0.044 Uiso 1 1 calc R
C7 C 0.5995(3) 0.2949(3) 1.1245(4) 0.0351(15) Uani 1 1 d .
C8 C 0.5286(4) 0.2553(3) 1.1220(6) 0.048(2) Uani 1 1 d .
C9 C 0.4289(4) 0.2391(4) 1.1460(9) 0.107(4) Uani 1 1 d .
H9A H 0.4113 0.2602 1.1073 0.128 Uiso 1 1 calc R
H9B H 0.4049 0.2257 1.2046 0.128 Uiso 1 1 calc R
C10 C 0.4256(4) 0.1817(4) 1.0953(8) 0.077(3) Uani 1 1 d .
H10A H 0.4033 0.1425 1.1331 0.093 Uiso 1 1 calc R
H10B H 0.4033 0.1743 1.0356 0.093 Uiso 1 1 calc R
C11 C 0.3950(4) 0.0585(4) 0.8816(7) 0.061(2) Uani 1 1 d .
C12 C 0.3440(4) 0.0254(5) 0.8138(8) 0.073(3) Uani 1 1 d .
H12A H 0.3196 -0.0200 0.8290 0.110 Uiso 1 1 calc R
H12B H 0.3626 0.0307 0.7523 0.110 Uiso 1 1 calc R
H12C H 0.3157 0.0434 0.8147 0.110 Uiso 1 1 calc R
O1 O 0.6752(3) 0.1872(3) 0.8312(4) 0.0677(15) Uani 1 1 d .
O2 O 0.4970(3) 0.2816(3) 1.1628(5) 0.076(2) Uani 1 1 d .
O3 O 0.5093(5) -0.0042(4) 1.2269(7) 0.148(4) Uani 1 1 d .
O4 O 0.5090(4) 0.0540(4) 1.1057(8) 0.150(3) Uani 1 1 d .
O5 O 0.5812(5) 0.0996(5) 1.2129(7) 0.173(4) Uani 1 1 d .
O6 O 0.5885(4) 0.0277(4) 1.1211(5) 0.133(3) Uani 1 1 d .
N1 N 0.5889(3) 0.1552(3) 0.9241(4) 0.0481(15) Uani 1 1 d .
N2 N 0.4948(3) 0.2008(3) 1.0812(5) 0.0468(15) Uani 1 1 d .
N3 N 0.4334(3) 0.0845(4) 0.9360(6) 0.081(2) 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
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'
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'
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'
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
N2 Cu1 N1 145.8(2) . .
N2 Cu1 N3 104.6(3) . .
N1 Cu1 N3 106.7(3) . .
O3 Cl1 O5 111.0(7) . .
O3 Cl1 O4 110.9(6) . .
O5 Cl1 O4 104.0(7) . .
O3 Cl1 O6 110.7(5) . .
O5 Cl1 O6 108.8(6) . .
O4 Cl1 O6 111.3(6) . .
C2 C1 C2 121.0(7) 2_655 .
C2 C1 H1A 119.5 2_655 .
C2 C1 H1A 119.5 . .
C1 C2 C1 119.0(7) 3_665 .
C1 C2 C3 121.1(7) 3_665 .
C1 C2 C3 119.8(7) . .
N1 C3 O1 118.2(7) . .
N1 C3 C2 126.7(7) . .
O1 C3 C2 115.1(7) . .
O1 C4 C5 104.5(6) . .
O1 C4 H4A 110.9 . .
C5 C4 H4A 110.9 . .
O1 C4 H4B 110.9 . .
C5 C4 H4B 110.9 . .
H4A C4 H4B 108.9 . .
N1 C5 C4 103.6(6) . .
N1 C5 H5A 111.0 . .
C4 C5 H5A 111.0 . .
N1 C5 H5B 111.0 . .
C4 C5 H5B 111.0 . .
H5A C5 H5B 109.0 . .
C7 C6 C7 121.5(7) . 2_655
C7 C6 H6A 119.2 . .
C7 C6 H6A 119.2 2_655 .
C6 C7 C6 118.5(7) . 3_665
C6 C7 C8 121.6(6) . .
C6 C7 C8 120.0(6) 3_665 .
N2 C8 O2 117.5(7) . .
N2 C8 C7 127.0(6) . .
O2 C8 C7 115.4(7) . .
O2 C9 C10 104.3(7) . .
O2 C9 H9A 110.9 . .
C10 C9 H9A 110.9 . .
O2 C9 H9B 110.9 . .
C10 C9 H9B 110.9 . .
H9A C9 H9B 108.9 . .
N2 C10 C9 103.8(6) . .
N2 C10 H10A 111.0 . .
C9 C10 H10A 111.0 . .
N2 C10 H10B 111.0 . .
C9 C10 H10B 111.0 . .
H10A C10 H10B 109.0 . .
N3 C11 C12 177.9(10) . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C3 O1 C4 106.5(6) . .
C8 O2 C9 107.4(7) . .
C3 N1 C5 107.1(6) . .
C3 N1 Cu1 131.2(5) . .
C5 N1 Cu1 121.6(5) . .
C8 N2 C10 106.7(6) . .
C8 N2 Cu1 131.1(5) . .
C10 N2 Cu1 121.4(5) . .
C11 N3 Cu1 160.2(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N2 1.927(6) .
Cu1 N1 1.929(6) .
Cu1 N3 2.068(8) .
Cl1 O3 1.317(8) .
Cl1 O5 1.349(9) .
Cl1 O4 1.369(8) .
Cl1 O6 1.388(7) .
C1 C2 1.377(8) 2_655
C1 C2 1.381(8) .
C1 H1A 0.9300 .
C2 C1 1.377(8) 3_665
C2 C3 1.465(9) .
C3 N1 1.258(9) .
C3 O1 1.339(9) .
C4 O1 1.446(9) .
C4 C5 1.515(12) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 N1 1.488(9) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 C7 1.365(8) .
C6 C7 1.386(8) 2_655
C6 H6A 0.9300 .
C7 C6 1.386(8) 3_665
C7 C8 1.463(9) .
C8 N2 1.273(9) .
C8 O2 1.325(8) .
C9 O2 1.436(9) .
C9 C10 1.509(12) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 N2 1.484(9) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 N3 1.118(9) .
C11 C12 1.436(12) .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
