#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:48:11 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180356 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/25/7202568.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_7202568
loop_
_publ_author_name
'Wang, Chuan-Feng'
'Zhu, Zhen-Yu'
'Zhang, Zheng-Xing'
'Chen, Zhen-Xia'
'Zhou, Xi-Geng'
_publ_section_title
;
 Crystal engineering of zinc(ii) and copper(ii) complexes containing
 3,5-dimethylisoxazole-4-carboxylate ligand via O?H?N, C?H?A (A = N, O
 and ?) and bifurcated C?H?N/O interactions
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              35
_journal_paper_doi               10.1039/b615091h
_journal_volume                  9
_journal_year                    2007
_chemical_formula_sum            'C36 H40 N6 O20 Zn3'
_chemical_formula_weight         1072.85
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.961(9)
_cell_angle_beta                 69.655(9)
_cell_angle_gamma                89.692(9)
_cell_formula_units_Z            1
_cell_length_a                   10.122(7)
_cell_length_b                   10.124(7)
_cell_length_c                   11.446(8)
_cell_measurement_temperature    298(2)
_cell_volume                     1099.6(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0225
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4591
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    1.709
_exptl_absorpt_correction_T_max  0.9194
_exptl_absorpt_correction_T_min  0.8477
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.0006(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         3790
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0297
_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)+(0.0639P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0864
_reflns_number_gt                3369
_reflns_number_total             3790
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b615091h.txt
_cod_data_source_block           f51021b
_cod_original_cell_volume        1099.5(14)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7202568
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_assembly
_atom_site_disorder_group
Zn1 Zn 0.0000 0.0000 0.0000 0.02654(12) Uani 1 2 d S . .
Zn2 Zn 0.12593(2) 0.20104(2) 0.18624(2) 0.02962(12) Uani 1 1 d . . .
N1 N -0.5263(2) 0.3017(2) 0.2804(2) 0.0507(6) Uani 1 1 d . . .
N2 N 0.0980(2) -0.4195(2) 0.3183(2) 0.0457(5) Uani 1 1 d . . .
N3 N 0.4991(2) 0.2395(3) -0.3935(2) 0.0540(6) Uani 1 1 d . . .
O1 O -0.13552(16) 0.10905(16) 0.14661(15) 0.0389(4) Uani 1 1 d . . .
O2 O -0.05613(16) 0.28339(16) 0.21665(16) 0.0381(4) Uani 1 1 d . . .
O3 O -0.47820(17) 0.39874(19) 0.34270(18) 0.0508(5) Uani 1 1 d . . .
O4 O 0.11969(17) -0.07748(16) 0.09904(15) 0.0378(4) Uani 1 1 d . . .
O5 O 0.12753(18) 0.02946(15) 0.26428(15) 0.0402(4) Uani 1 1 d . . .
O6 O 0.11177(19) -0.35019(17) 0.41898(17) 0.0466(4) Uani 1 1 d . . .
O7 O 0.13851(16) 0.15406(16) -0.08044(16) 0.0404(4) Uani 1 1 d . . .
O8 O 0.26784(17) 0.23245(18) 0.02445(15) 0.0456(4) Uani 1 1 d . . .
O9 O 0.5678(2) 0.3086(2) -0.3238(2) 0.0703(6) Uani 1 1 d . . .
O10 O 0.1886(2) 0.31436(19) 0.29837(18) 0.0428(4) Uani 1 1 d . . .
C1 C -0.1522(2) 0.2184(2) 0.1976(2) 0.0303(5) Uani 1 1 d . . .
C2 C -0.2953(2) 0.2740(2) 0.2440(2) 0.0324(5) Uani 1 1 d . . .
C3 C -0.4175(2) 0.2289(2) 0.2232(2) 0.0398(6) Uani 1 1 d . . .
C4 C -0.3404(2) 0.3805(2) 0.3189(2) 0.0371(5) Uani 1 1 d . . .
C5 C -0.4363(3) 0.1151(3) 0.1493(3) 0.0571(8) Uani 1 1 d . . .
H5A H -0.4261 0.0338 0.1899 0.086 Uiso 1 1 calc R . .
H5B H -0.3664 0.1194 0.0673 0.086 Uiso 1 1 calc R . .
H5C H -0.5285 0.1188 0.1433 0.086 Uiso 1 1 calc R . .
C6 C -0.2727(3) 0.4735(3) 0.3779(3) 0.0497(7) Uani 1 1 d . . .
H6A H -0.2223 0.5394 0.3178 0.075 Uiso 1 1 calc R . .
H6B H -0.2083 0.4265 0.4083 0.075 Uiso 1 1 calc R . .
H6C H -0.3434 0.5155 0.4461 0.075 Uiso 1 1 calc R . .
C7 C 0.1209(2) -0.0754(2) 0.2066(2) 0.0302(5) Uani 1 1 d . . .
C8 C 0.1165(2) -0.2017(2) 0.2739(2) 0.0334(5) Uani 1 1 d . . .
C9 C 0.1007(3) -0.3320(2) 0.2334(2) 0.0381(5) Uani 1 1 d . . .
C10 C 0.1238(2) -0.2211(2) 0.3892(2) 0.0371(5) Uani 1 1 d . . .
C11 C 0.0924(3) -0.3759(3) 0.1130(3) 0.0559(7) Uani 1 1 d . . .
H11A H 0.0817 -0.4702 0.1152 0.084 Uiso 1 1 calc R . .
H11B H 0.1772 -0.3511 0.0464 0.084 Uiso 1 1 calc R . .
H11C H 0.0129 -0.3349 0.0997 0.084 Uiso 1 1 calc R . .
C12 C 0.1458(3) -0.1333(3) 0.4825(2) 0.0518(7) Uani 1 1 d . . .
H12A H 0.0565 -0.1127 0.5446 0.078 Uiso 1 1 calc R . .
H12B H 0.1907 -0.0531 0.4421 0.078 Uiso 1 1 calc R . .
H12C H 0.2046 -0.1768 0.5214 0.078 Uiso 1 1 calc R . .
C13 C 0.2470(2) 0.2049(2) -0.0751(2) 0.0340(5) Uani 1 1 d . . .
C14 C 0.3626(2) 0.2370(2) -0.1925(2) 0.0380(5) Uani 1 1 d . . .
C15 C 0.3778(3) 0.1989(3) -0.3136(2) 0.0482(6) Uani 1 1 d . . .
C16 C 0.4841(3) 0.3065(3) -0.2059(3) 0.0481(6) Uani 1 1 d . . .
C17 C 0.2847(4) 0.1268(4) -0.3639(3) 0.0754(10) Uani 1 1 d . . .
H17A H 0.3368 0.1009 -0.4476 0.113 Uiso 1 1 calc R . .
H17B H 0.2078 0.1828 -0.3638 0.113 Uiso 1 1 calc R . .
H17C H 0.2485 0.0496 -0.3131 0.113 Uiso 1 1 calc R . .
C18 C 0.5310(4) 0.3768(4) -0.1159(3) 0.0754(10) Uani 1 1 d . . .
H18A H 0.5706 0.3147 -0.0728 0.113 Uiso 1 1 calc R . .
H18B H 0.4520 0.4203 -0.0568 0.113 Uiso 1 1 calc R . .
H18C H 0.6010 0.4412 -0.1592 0.113 Uiso 1 1 calc R . .
H10A H 0.277(4) 0.319(3) 0.301(3) 0.077(11) Uiso 1 1 d . . .
H10B H 0.171(3) 0.396(3) 0.301(3) 0.052(9) Uiso 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'
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
_geom_angle_publ_flag
O4 Zn1 O4 180.00(10) 2 . ?
O4 Zn1 O7 94.73(8) 2 2 ?
O4 Zn1 O7 85.27(8) . 2 ?
O4 Zn1 O7 85.27(8) 2 . ?
O4 Zn1 O7 94.73(8) . . ?
O7 Zn1 O7 180.00(11) 2 . ?
O4 Zn1 O1 84.06(8) 2 . ?
O4 Zn1 O1 95.94(8) . . ?
O7 Zn1 O1 83.88(8) 2 . ?
O7 Zn1 O1 96.12(8) . . ?
O4 Zn1 O1 95.94(8) 2 2 ?
O4 Zn1 O1 84.06(8) . 2 ?
O7 Zn1 O1 96.12(8) 2 2 ?
O7 Zn1 O1 83.88(8) . 2 ?
O1 Zn1 O1 180.0 . 2 ?
O8 Zn2 O2 116.82(8) . . ?
O8 Zn2 O5 116.93(8) . . ?
O2 Zn2 O5 117.15(7) . . ?
O8 Zn2 O10 103.33(9) . . ?
O2 Zn2 O10 97.30(8) . . ?
O5 Zn2 O10 99.79(9) . . ?
C3 N1 O3 106.21(19) . . ?
C9 N2 O6 106.7(2) . . ?
C15 N3 O9 106.6(2) . . ?
C1 O1 Zn1 143.61(15) . . ?
C1 O2 Zn2 119.00(15) . . ?
C4 O3 N1 108.69(18) . . ?
C7 O4 Zn1 138.01(15) . . ?
C7 O5 Zn2 119.88(15) . . ?
C10 O6 N2 108.48(18) . . ?
C13 O7 Zn1 140.09(16) . . ?
C13 O8 Zn2 121.74(15) . . ?
C16 O9 N3 107.9(2) . . ?
O1 C1 O2 124.8(2) . . ?
O1 C1 C2 118.02(19) . . ?
O2 C1 C2 117.2(2) . . ?
C4 C2 C3 104.4(2) . . ?
C4 C2 C1 127.3(2) . . ?
C3 C2 C1 128.3(2) . . ?
N1 C3 C2 111.2(2) . . ?
N1 C3 C5 118.7(2) . . ?
C2 C3 C5 130.1(2) . . ?
O3 C4 C2 109.5(2) . . ?
O3 C4 C6 115.9(2) . . ?
C2 C4 C6 134.6(2) . . ?
O4 C7 O5 124.5(2) . . ?
O4 C7 C8 118.7(2) . . ?
O5 C7 C8 116.8(2) . . ?
C10 C8 C9 104.2(2) . . ?
C10 C8 C7 127.9(2) . . ?
C9 C8 C7 127.8(2) . . ?
N2 C9 C8 110.8(2) . . ?
N2 C9 C11 119.3(2) . . ?
C8 C9 C11 129.9(2) . . ?
O6 C10 C8 109.8(2) . . ?
O6 C10 C12 115.9(2) . . ?
C8 C10 C12 134.2(2) . . ?
O7 C13 O8 125.0(2) . . ?
O7 C13 C14 118.7(2) . . ?
O8 C13 C14 116.3(2) . . ?
C16 C14 C15 104.7(2) . . ?
C16 C14 C13 127.0(2) . . ?
C15 C14 C13 128.3(2) . . ?
N3 C15 C14 110.7(3) . . ?
N3 C15 C17 117.1(3) . . ?
C14 C15 C17 132.2(3) . . ?
O9 C16 C14 110.1(3) . . ?
O9 C16 C18 117.8(2) . . ?
C14 C16 C18 132.0(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O4 2.0690(18) 2 ?
Zn1 O4 2.0690(18) . ?
Zn1 O7 2.0784(18) 2 ?
Zn1 O7 2.0784(18) . ?
Zn1 O1 2.0896(18) . ?
Zn1 O1 2.0896(18) 2 ?
Zn2 O8 1.9307(19) . ?
Zn2 O2 1.9391(19) . ?
Zn2 O5 1.9415(19) . ?
Zn2 O10 1.9980(19) . ?
N1 C3 1.301(3) . ?
N1 O3 1.408(3) . ?
N2 C9 1.296(3) . ?
N2 O6 1.407(3) . ?
N3 C15 1.313(3) . ?
N3 O9 1.421(3) . ?
O1 C1 1.244(3) . ?
O2 C1 1.259(3) . ?
O3 C4 1.338(3) . ?
O4 C7 1.236(3) . ?
O5 C7 1.274(3) . ?
O6 C10 1.340(3) . ?
O7 C13 1.236(3) . ?
O8 C13 1.265(3) . ?
O9 C16 1.320(3) . ?
C1 C2 1.471(3) . ?
C2 C4 1.365(3) . ?
C2 C3 1.418(3) . ?
C3 C5 1.493(4) . ?
C4 C6 1.470(4) . ?
C7 C8 1.473(3) . ?
C8 C10 1.358(3) . ?
C8 C9 1.434(3) . ?
C9 C11 1.486(4) . ?
C10 C12 1.478(4) . ?
C13 C14 1.475(3) . ?
C14 C16 1.380(4) . ?
C14 C15 1.401(4) . ?
C15 C17 1.467(4) . ?
C16 C18 1.471(5) . ?
