#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/26/7212653.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_7212653
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_moiety         'C34 H40 Cl2 Cu2 N8 O16'
_chemical_formula_sum            'C34 H40 Cl2 Cu2 N8 O16'
_chemical_formula_weight         1014.72
_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                118.6290(10)
_cell_angle_beta                 93.0040(10)
_cell_angle_gamma                99.6650(10)
_cell_formula_units_Z            1
_cell_length_a                   7.0086(6)
_cell_length_b                   12.9662(11)
_cell_length_c                   13.0105(11)
_cell_measurement_reflns_used    2108
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.64
_cell_measurement_theta_min      2.48
_cell_volume                     1010.92(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker Smart Apec CCD'
_diffrn_measurement_method       'ω and φ 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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5092
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    1.267
_exptl_absorpt_correction_T_max  0.9279
_exptl_absorpt_correction_T_min  0.7593
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         3525
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0449
_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)+(0.0650P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1148
_reflns_number_gt                2810
_reflns_number_total             3525
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c002874f.txt
_cod_data_source_block           4
_cod_original_sg_symbol_Hall     '-p 1'
_cod_original_sg_symbol_H-M      'p -1'
_cod_database_code               7212653
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
Cu1 Cu 0.58447(6) 0.47452(4) 0.29589(4) 0.04771(18) Uani 1 1 d . . .
Cl1 Cl 0.79531(16) 0.09956(9) 0.30011(10) 0.0672(3) Uani 1 1 d . . .
O1 O 0.1896(4) 0.17573(19) 0.0349(2) 0.0518(6) Uani 1 1 d . . .
O1W O 0.8608(5) 0.3439(3) 0.1966(3) 0.0713(9) Uani 1 1 d . . .
O2 O 0.2159(4) 0.1861(2) -0.3385(2) 0.0564(7) Uani 1 1 d . . .
O3 O 0.2739(4) 0.72038(19) 0.21474(19) 0.0533(6) Uani 1 1 d . . .
O4 O 0.8908(6) 0.2156(3) 0.3299(3) 0.0961(11) Uani 1 1 d . A .
O5 O 0.6824(7) 0.0469(5) 0.1871(4) 0.192(3) Uani 1 1 d . A .
O6 O 0.9370(7) 0.0326(3) 0.2857(4) 0.1313(16) Uani 1 1 d . A .
O7 O 0.714(6) 0.1020(10) 0.395(3) 0.172(10) Uani 0.72(6) 1 d P A 1
O7' O 0.634(3) 0.123(3) 0.3617(17) 0.075(11) Uani 0.28(6) 1 d P A 2
N1 N 0.3830(4) 0.3306(2) 0.1938(2) 0.0375(6) Uani 1 1 d . . .
N2 N 0.3189(4) 0.3579(2) -0.3385(2) 0.0387(6) Uani 1 1 d . . .
N3 N 0.2375(4) 0.7350(2) 0.0510(2) 0.0448(7) Uani 1 1 d . . .
N4 N 0.6932(5) 0.4617(3) 0.4399(3) 0.0567(8) Uani 1 1 d . . .
C1 C 0.2718(4) 0.3564(3) 0.0278(3) 0.0330(7) Uani 1 1 d . . .
C2 C 0.2628(4) 0.2984(3) -0.0939(3) 0.0342(7) Uani 1 1 d . . .
H2A H 0.2614 0.2165 -0.1360 0.041 Uiso 1 1 calc R . .
C3 C 0.2558(4) 0.3633(3) -0.1525(3) 0.0344(7) Uani 1 1 d . . .
C4 C 0.2490(4) 0.4835(3) -0.0900(3) 0.0347(7) Uani 1 1 d . . .
H4A H 0.2395 0.5260 -0.1301 0.042 Uiso 1 1 calc R . .
C5 C 0.2561(4) 0.5412(3) 0.0312(3) 0.0326(7) Uani 1 1 d . . .
C6 C 0.2691(4) 0.4772(3) 0.0901(3) 0.0345(7) Uani 1 1 d . . .
H6A H 0.2762 0.5157 0.1721 0.041 Uiso 1 1 calc R . .
C7 C 0.2880(5) 0.2902(3) 0.0923(3) 0.0369(7) Uani 1 1 d . . .
C8 C 0.3439(6) 0.2325(3) 0.2228(3) 0.0533(9) Uani 1 1 d . . .
H8A H 0.2617 0.2507 0.2843 0.064 Uiso 1 1 calc R . .
H8B H 0.4650 0.2190 0.2488 0.064 Uiso 1 1 calc R . .
C9 C 0.2402(7) 0.1254(3) 0.1080(3) 0.0676(12) Uani 1 1 d . . .
H9A H 0.3254 0.0701 0.0719 0.081 Uiso 1 1 calc R . .
H9B H 0.1236 0.0829 0.1201 0.081 Uiso 1 1 calc R . .
C10 C 0.2652(5) 0.3056(3) -0.2805(3) 0.0386(7) Uani 1 1 d . . .
C11 C 0.3020(6) 0.2616(3) -0.4637(3) 0.0516(9) Uani 1 1 d . . .
H11A H 0.4251 0.2675 -0.4934 0.062 Uiso 1 1 calc R . .
H11B H 0.2006 0.2664 -0.5138 0.062 Uiso 1 1 calc R . .
C12 C 0.2494(8) 0.1465(3) -0.4594(3) 0.0738(13) Uani 1 1 d . . .
H12A H 0.1323 0.0938 -0.5151 0.089 Uiso 1 1 calc R . .
H12B H 0.3557 0.1043 -0.4773 0.089 Uiso 1 1 calc R . .
C13 C 0.2533(4) 0.6700(3) 0.0966(3) 0.0371(7) Uani 1 1 d . . .
C14 C 0.2450(6) 0.8565(3) 0.1492(3) 0.0585(10) Uani 1 1 d . . .
H14A H 0.1238 0.8814 0.1433 0.070 Uiso 1 1 calc R . .
H14B H 0.3528 0.9143 0.1493 0.070 Uiso 1 1 calc R . .
C15 C 0.2743(6) 0.8469(3) 0.2585(3) 0.0609(10) Uani 1 1 d . . .
H15A H 0.3980 0.8979 0.3076 0.073 Uiso 1 1 calc R . .
H15B H 0.1690 0.8700 0.3045 0.073 Uiso 1 1 calc R . .
C16 C 0.7590(5) 0.4421(3) 0.5071(3) 0.0453(8) Uani 1 1 d . . .
C17 C 0.8444(7) 0.4160(4) 0.5933(4) 0.0597(11) Uani 1 1 d D . .
H1WA H 0.832(6) 0.304(4) 0.126(4) 0.068(15) Uiso 1 1 d . . .
H17A H 0.905(5) 0.490(3) 0.659(3) 0.074(13) Uiso 1 1 d D . .
H17B H 0.745(6) 0.375(3) 0.612(4) 0.13(2) Uiso 1 1 d D . .
H1WB H 0.856(7) 0.296(4) 0.210(4) 0.074(17) Uiso 1 1 d . . .
H17C H 0.940(5) 0.372(3) 0.562(4) 0.13(2) Uiso 1 1 d 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
N1 Cu1 N2 143.64(11) . 2_665
N1 Cu1 N4 108.69(11) . .
N2 Cu1 N4 105.20(11) 2_665 .
O7 Cl1 O6 104(2) . .
O7 Cl1 O4 109.6(5) . .
O6 Cl1 O4 107.6(3) . .
O7 Cl1 O5 121.5(19) . .
O6 Cl1 O5 105.5(3) . .
O4 Cl1 O5 107.6(3) . .
O7 Cl1 O7' 35.4(10) . .
O6 Cl1 O7' 137.7(16) . .
O4 Cl1 O7' 100.9(13) . .
O5 Cl1 O7' 94.5(9) . .
C7 O1 C9 105.6(3) . .
H1WA O1W H1WB 98(5) . .
C10 O2 C12 106.9(3) . .
C13 O3 C15 105.4(3) . .
C7 N1 C8 106.6(3) . .
C7 N1 Cu1 133.3(2) . .
C8 N1 Cu1 119.29(19) . .
C10 N2 C11 106.5(3) . .
C10 N2 Cu1 134.1(2) . 2_665
C11 N2 Cu1 119.4(2) . 2_665
C13 N3 C14 106.6(3) . .
C16 N4 Cu1 171.1(3) . .
C6 C1 C2 120.4(3) . .
C6 C1 C7 119.5(3) . .
C2 C1 C7 120.1(3) . .
C1 C2 C3 119.3(3) . .
C1 C2 H2A 120.3 . .
C3 C2 H2A 120.3 . .
C4 C3 C2 119.9(3) . .
C4 C3 C10 120.1(3) . .
C2 C3 C10 119.9(3) . .
C5 C4 C3 120.8(3) . .
C5 C4 H4A 119.6 . .
C3 C4 H4A 119.6 . .
C4 C5 C6 119.2(3) . .
C4 C5 C13 120.0(3) . .
C6 C5 C13 120.8(3) . .
C1 C6 C5 120.3(3) . .
C1 C6 H6A 119.9 . .
C5 C6 H6A 119.9 . .
N1 C7 O1 118.2(3) . .
N1 C7 C1 127.0(3) . .
O1 C7 C1 114.8(3) . .
N1 C8 C9 103.5(3) . .
N1 C8 H8A 111.1 . .
C9 C8 H8A 111.1 . .
N1 C8 H8B 111.1 . .
C9 C8 H8B 111.1 . .
H8A C8 H8B 109.0 . .
O1 C9 C8 104.4(3) . .
O1 C9 H9A 110.9 . .
C8 C9 H9A 110.9 . .
O1 C9 H9B 110.9 . .
C8 C9 H9B 110.9 . .
H9A C9 H9B 108.9 . .
N2 C10 O2 117.9(3) . .
N2 C10 C3 126.8(3) . .
O2 C10 C3 115.2(3) . .
N2 C11 C12 104.2(3) . .
N2 C11 H11A 110.9 . .
C12 C11 H11A 110.9 . .
N2 C11 H11B 110.9 . .
C12 C11 H11B 110.9 . .
H11A C11 H11B 108.9 . .
O2 C12 C11 103.9(3) . .
O2 C12 H12A 111.0 . .
C11 C12 H12A 111.0 . .
O2 C12 H12B 111.0 . .
C11 C12 H12B 111.0 . .
H12A C12 H12B 109.0 . .
N3 C13 O3 118.7(3) . .
N3 C13 C5 125.5(3) . .
O3 C13 C5 115.8(3) . .
N3 C14 C15 104.9(3) . .
N3 C14 H14A 110.8 . .
C15 C14 H14A 110.8 . .
N3 C14 H14B 110.8 . .
C15 C14 H14B 110.8 . .
H14A C14 H14B 108.8 . .
O3 C15 C14 104.4(3) . .
O3 C15 H15A 110.9 . .
C14 C15 H15A 110.9 . .
O3 C15 H15B 110.9 . .
C14 C15 H15B 110.9 . .
H15A C15 H15B 108.9 . .
N4 C16 C17 179.6(4) . .
C16 C17 H17A 107(2) . .
C16 C17 H17B 108(4) . .
H17A C17 H17B 112(2) . .
C16 C17 H17C 109(3) . .
H17A C17 H17C 108(2) . .
H17B C17 H17C 112(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 1.946(2) .
Cu1 N2 1.949(3) 2_665
Cu1 N4 2.076(3) .
Cl1 O7 1.381(18) .
Cl1 O6 1.388(4) .
Cl1 O4 1.392(3) .
Cl1 O5 1.410(4) .
Cl1 O7' 1.41(2) .
O1 C7 1.333(4) .
O1 C9 1.447(4) .
O1W H1WA 0.80(4) .
O1W H1WB 0.73(4) .
O2 C10 1.328(4) .
O2 C12 1.448(4) .
O3 C13 1.339(4) .
O3 C15 1.456(4) .
N1 C7 1.261(4) .
N1 C8 1.480(4) .
N2 C10 1.267(4) .
N2 C11 1.486(4) .
N2 Cu1 1.949(3) 2_665
N3 C13 1.257(4) .
N3 C14 1.468(4) .
N4 C16 1.120(4) .
C1 C6 1.380(4) .
C1 C2 1.381(4) .
C1 C7 1.472(4) .
C2 C3 1.386(4) .
C2 H2A 0.9300 .
C3 C4 1.381(4) .
C3 C10 1.473(4) .
C4 C5 1.377(4) .
C4 H4A 0.9300 .
C5 C6 1.383(4) .
C5 C13 1.471(4) .
C6 H6A 0.9300 .
C8 C9 1.499(5) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C11 C12 1.505(5) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C14 C15 1.492(5) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C16 C17 1.446(5) .
C17 H17A 0.93(3) .
C17 H17B 0.92(3) .
C17 H17C 0.93(3) .
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
O1W H1WA N3 0.80(4) 2.12(4) 2.876(5) 158(4) 2_665
O1W H1WB O4 0.73(4) 2.27(5) 2.943(5) 155(5) .
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
N2 Cu1 N1 C7 30.1(4) 2_665
N4 Cu1 N1 C7 -172.1(3) .
N2 Cu1 N1 C8 -162.1(2) 2_665
N4 Cu1 N1 C8 -4.3(3) .
N1 Cu1 N4 C16 61(2) .
N2 Cu1 N4 C16 -131.9(19) 2_665
C6 C1 C2 C3 1.5(4) .
C7 C1 C2 C3 -177.3(3) .
C1 C2 C3 C4 -2.9(4) .
C1 C2 C3 C10 174.2(3) .
C2 C3 C4 C5 2.3(4) .
C10 C3 C4 C5 -174.7(3) .
C3 C4 C5 C6 -0.4(4) .
C3 C4 C5 C13 178.6(3) .
C2 C1 C6 C5 0.4(4) .
C7 C1 C6 C5 179.3(3) .
C4 C5 C6 C1 -1.0(4) .
C13 C5 C6 C1 -180.0(3) .
C8 N1 C7 O1 -3.3(4) .
Cu1 N1 C7 O1 165.6(2) .
C8 N1 C7 C1 176.5(3) .
Cu1 N1 C7 C1 -14.6(5) .
C9 O1 C7 N1 -5.5(4) .
C9 O1 C7 C1 174.7(3) .
C6 C1 C7 N1 -34.5(5) .
C2 C1 C7 N1 144.4(3) .
C6 C1 C7 O1 145.3(3) .
C2 C1 C7 O1 -35.8(4) .
C7 N1 C8 C9 10.2(4) .
Cu1 N1 C8 C9 -160.6(3) .
C7 O1 C9 C8 11.4(4) .
N1 C8 C9 O1 -12.9(4) .
C11 N2 C10 O2 2.0(4) .
Cu1 N2 C10 O2 -176.5(2) 2_665
C11 N2 C10 C3 -179.7(3) .
Cu1 N2 C10 C3 1.8(5) 2_665
C12 O2 C10 N2 3.0(4) .
C12 O2 C10 C3 -175.5(3) .
C4 C3 C10 N2 20.0(5) .
C2 C3 C10 N2 -157.1(3) .
C4 C3 C10 O2 -161.7(3) .
C2 C3 C10 O2 21.2(4) .
C10 N2 C11 C12 -5.9(4) .
Cu1 N2 C11 C12 172.9(3) 2_665
C10 O2 C12 C11 -6.4(4) .
N2 C11 C12 O2 7.3(4) .
C14 N3 C13 O3 -0.6(4) .
C14 N3 C13 C5 -179.0(3) .
C15 O3 C13 N3 -0.8(4) .
C15 O3 C13 C5 177.8(3) .
C4 C5 C13 N3 2.8(5) .
C6 C5 C13 N3 -178.3(3) .
C4 C5 C13 O3 -175.7(3) .
C6 C5 C13 O3 3.2(4) .
C13 N3 C14 C15 1.7(4) .
C13 O3 C15 C14 1.8(4) .
N3 C14 C15 O3 -2.1(4) .
Cu1 N4 C16 C17 2(65) .
