#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:36:37 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180441 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/10/7211036.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_7211036
loop_
_publ_author_name
'He, Zhi'
'Pang, Qingqing'
'Rankine, Damien'
'Sumby, Christopher J.'
'Zhang, Lijuan'
'Doonan, Christian J.'
'Li, Qiaowei'
_publ_section_title
;
 Encapsulation of polyoxometalates within layered metal--organic
 frameworks with topological and pore control
;
_journal_issue                   45
_journal_name_full               CrystEngComm
_journal_page_first              9340
_journal_paper_doi               10.1039/c3ce41136b
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C24 H21 Cu N O5'
_chemical_formula_weight         466.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 113.821(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.26(4)
_cell_length_b                   9.821(14)
_cell_length_c                   18.95(3)
_cell_measurement_reflns_used    671
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.23
_cell_measurement_theta_min      1.96
_cell_volume                     4982(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0925
_diffrn_reflns_av_sigmaI/netI    0.1261
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11170
_diffrn_reflns_theta_full        24.81
_diffrn_reflns_theta_max         24.81
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.908
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.033
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.707
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.707
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.0582
_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2105
_refine_ls_wR_factor_ref         0.2320
_reflns_number_gt                2171
_reflns_number_total             4211
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41136b.txt
_cod_data_source_block           ql_hz45_2_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        4981(13)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7211036
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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 0.23757(2) 0.65806(7) 0.04035(4) 0.0434(3) Uani 1 1 d . . .
O1 O 0.18607(15) 0.7907(5) 0.0358(3) 0.0579(12) Uani 1 1 d . . .
O2 O 0.29323(16) 0.5533(5) 0.0332(3) 0.0609(13) Uani 1 1 d . . .
O3 O 0.28728(16) 0.7563(5) 0.1297(3) 0.0633(13) Uani 1 1 d . . .
O4 O 0.19201(17) 0.5845(5) -0.0601(3) 0.0613(12) Uani 1 1 d . . .
O5 O 0.2230(3) 0.5035(9) 0.1092(5) 0.099(2) Uani 1 1 d . . .
C1 C 0.1388(2) 0.9958(6) -0.0004(4) 0.0499(16) Uani 1 1 d . . .
C2 C 0.1276(2) 1.1169(7) -0.0414(4) 0.0601(19) Uani 1 1 d . . .
H2 H 0.1469 1.1444 -0.0676 0.072 Uiso 1 1 calc R . .
C3 C 0.0885(2) 1.1972(7) -0.0441(4) 0.0611(19) Uani 1 1 d . . .
H3 H 0.0816 1.2771 -0.0729 0.073 Uiso 1 1 calc R . .
C4 C 0.0589(2) 1.1612(6) -0.0045(4) 0.0511(16) Uani 1 1 d . . .
C5 C 0.0706(2) 1.0411(7) 0.0396(4) 0.0571(17) Uani 1 1 d . . .
H5 H 0.0519 1.0164 0.0673 0.068 Uiso 1 1 calc R . .
C6 C 0.1100(2) 0.9588(7) 0.0419(4) 0.0553(17) Uani 1 1 d . . .
H6 H 0.1175 0.8793 0.0711 0.066 Uiso 1 1 calc R . .
C7 C 0.0147(2) 1.2451(6) -0.0094(4) 0.0504(16) Uani 1 1 d . . .
C8 C -0.0161(2) 1.3094(7) -0.0796(4) 0.0549(18) Uani 1 1 d . . .
H8 H -0.0082 1.3006 -0.1224 0.066 Uiso 1 1 calc R . .
C9 C -0.0578(2) 1.3856(6) -0.0860(4) 0.0501(16) Uani 1 1 d . . .
C10 C -0.0687(2) 1.3995(7) -0.0194(4) 0.0609(19) Uani 1 1 d . . .
H10 H -0.0963 1.4502 -0.0226 0.073 Uiso 1 1 calc R . .
C11 C -0.0388(3) 1.3385(7) 0.0505(4) 0.0627(19) Uani 1 1 d . . .
C12 C 0.0031(2) 1.2615(7) 0.0557(4) 0.0578(18) Uani 1 1 d . . .
H12 H 0.0233 1.2211 0.1024 0.069 Uiso 1 1 calc R . .
C13 C -0.0503(3) 1.3581(9) 0.1211(5) 0.094(3) Uani 1 1 d . . .
H13A H -0.0708 1.4377 0.1143 0.141 Uiso 1 1 calc R . .
H13B H -0.0197 1.3693 0.1659 0.141 Uiso 1 1 calc R . .
H13C H -0.0679 1.2798 0.1277 0.141 Uiso 1 1 calc R . .
C14 C -0.0904(2) 1.4505(7) -0.1597(4) 0.0513(16) Uani 1 1 d . . .
C15 C -0.0971(3) 1.3951(7) -0.2300(4) 0.064(2) Uani 1 1 d . . .
H15 H -0.0802 1.3152 -0.2305 0.077 Uiso 1 1 calc R . .
C16 C -0.1161(2) 1.5718(7) -0.1613(4) 0.0584(18) Uani 1 1 d . . .
H16 H -0.1124 1.6126 -0.1150 0.070 Uiso 1 1 calc R . .
C17 C -0.1465(2) 1.6317(6) -0.2294(4) 0.0581(18) Uani 1 1 d . . .
H17 H -0.1626 1.7127 -0.2281 0.070 Uiso 1 1 calc R . .
C18 C -0.1541(2) 1.5745(6) -0.3009(4) 0.0533(17) Uani 1 1 d . . .
C19 C -0.1282(2) 1.4532(7) -0.3009(4) 0.0624(18) Uani 1 1 d . . .
H19 H -0.1317 1.4124 -0.3471 0.075 Uiso 1 1 calc R . .
C20 C 0.1805(2) 0.9035(7) 0.0009(4) 0.0519(17) Uani 1 1 d . . .
C21 C -0.1890(2) 1.6380(7) -0.3770(5) 0.0548(18) Uani 1 1 d . . .
C22 C 0.2506(7) 0.459(3) 0.1641(12) 0.079(8) Uani 0.54(4) 1 d P A 1
H22 H 0.2723 0.5179 0.2006 0.095 Uiso 0.54(4) 1 calc PR A 1
C221 C 0.2287(10) 0.400(3) 0.121(2) 0.079(10) Uani 0.46(4) 1 d P A 2
H221 H 0.2105 0.3480 0.0777 0.095 Uiso 0.46(4) 1 calc PR A 2
C23 C 0.2887(6) 0.3032(17) 0.2638(8) 0.177(6) Uani 1 1 d . A .
H23A H 0.2912 0.3884 0.2899 0.265 Uiso 1 1 calc R . .
H23B H 0.3212 0.2764 0.2678 0.265 Uiso 1 1 calc R . .
H23C H 0.2758 0.2350 0.2870 0.265 Uiso 1 1 calc R . .
C24 C 0.2348(6) 0.1946(19) 0.1454(11) 0.215(8) Uani 1 1 d . A .
H24A H 0.2023 0.1815 0.1457 0.323 Uiso 1 1 calc R . .
H24B H 0.2563 0.1210 0.1724 0.323 Uiso 1 1 calc R . .
H24C H 0.2318 0.1969 0.0931 0.323 Uiso 1 1 calc R . .
N1 N 0.2550(3) 0.3185(8) 0.1820(5) 0.090(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'
O O 0.0106 0.0060 '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'
N N 0.0061 0.0033 '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 Cu1 O4 89.6(2) . .
O1 Cu1 O2 168.38(19) . .
O4 Cu1 O2 89.9(2) . .
O1 Cu1 O3 90.0(2) . .
O4 Cu1 O3 169.17(19) . .
O2 Cu1 O3 88.3(2) . .
O1 Cu1 O5 99.0(2) . .
O4 Cu1 O5 96.0(3) . .
O2 Cu1 O5 92.6(2) . .
O3 Cu1 O5 94.8(3) . .
O1 Cu1 Cu1 84.70(17) . 7_565
O4 Cu1 Cu1 85.90(18) . 7_565
O2 Cu1 Cu1 83.68(16) . 7_565
O3 Cu1 Cu1 83.28(18) . 7_565
O5 Cu1 Cu1 175.79(18) . 7_565
C20 O1 Cu1 122.5(4) . .
C20 O2 Cu1 123.3(4) 7_565 .
C21 O3 Cu1 123.3(5) 8_576 .
C21 O4 Cu1 121.2(4) 2_544 .
C221 O5 C22 54.6(16) . .
C221 O5 Cu1 140.1(14) . .
C22 O5 Cu1 126.5(13) . .
C2 C1 C6 118.3(6) . .
C2 C1 C20 122.1(6) . .
C6 C1 C20 119.6(6) . .
C3 C2 C1 121.3(6) . .
C3 C2 H2 119.4 . .
C1 C2 H2 119.4 . .
C2 C3 C4 121.4(6) . .
C2 C3 H3 119.3 . .
C4 C3 H3 119.3 . .
C3 C4 C5 118.4(6) . .
C3 C4 C7 122.1(6) . .
C5 C4 C7 119.5(6) . .
C6 C5 C4 120.3(6) . .
C6 C5 H5 119.9 . .
C4 C5 H5 119.9 . .
C5 C6 C1 120.3(6) . .
C5 C6 H6 119.8 . .
C1 C6 H6 119.8 . .
C12 C7 C8 119.0(6) . .
C12 C7 C4 120.7(6) . .
C8 C7 C4 120.3(6) . .
C9 C8 C7 121.4(6) . .
C9 C8 H8 119.3 . .
C7 C8 H8 119.3 . .
C8 C9 C10 118.3(6) . .
C8 C9 C14 121.3(6) . .
C10 C9 C14 120.3(6) . .
C11 C10 C9 121.4(6) . .
C11 C10 H10 119.3 . .
C9 C10 H10 119.3 . .
C10 C11 C12 119.6(6) . .
C10 C11 C13 120.3(6) . .
C12 C11 C13 120.2(7) . .
C11 C12 C7 120.4(6) . .
C11 C12 H12 119.8 . .
C7 C12 H12 119.8 . .
C11 C13 H13A 109.5 . .
C11 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C11 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C15 C14 C16 116.7(6) . .
C15 C14 C9 121.9(6) . .
C16 C14 C9 121.5(6) . .
C14 C15 C19 123.2(6) . .
C14 C15 H15 118.4 . .
C19 C15 H15 118.4 . .
C17 C16 C14 121.6(6) . .
C17 C16 H16 119.2 . .
C14 C16 H16 119.2 . .
C16 C17 C18 121.9(6) . .
C16 C17 H17 119.1 . .
C18 C17 H17 119.1 . .
C17 C18 C19 117.6(6) . .
C17 C18 C21 122.4(6) . .
C19 C18 C21 120.0(7) . .
C15 C19 C18 118.9(7) . .
C15 C19 H19 120.5 . .
C18 C19 H19 120.5 . .
O2 C20 O1 125.8(6) 7_565 .
O2 C20 C1 116.4(6) 7_565 .
O1 C20 C1 117.8(6) . .
O4 C21 O3 126.2(6) 2_564 8_475
O4 C21 C18 119.0(6) 2_564 .
O3 C21 C18 114.8(7) 8_475 .
O5 C22 N1 125(2) . .
O5 C22 H22 117.6 . .
N1 C22 H22 117.6 . .
O5 C221 N1 138(4) . .
O5 C221 H221 110.9 . .
N1 C221 H221 110.9 . .
N1 C23 H23A 109.5 . .
N1 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
N1 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
N1 C24 H24A 109.5 . .
N1 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
N1 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
C221 N1 C24 96.2(19) . .
C221 N1 C22 42.0(12) . .
C24 N1 C22 138.2(15) . .
C221 N1 C23 149.8(19) . .
C24 N1 C23 113.7(12) . .
C22 N1 C23 108.1(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.967(5) .
Cu1 O4 1.968(5) .
Cu1 O2 1.976(5) .
Cu1 O3 1.981(5) .
Cu1 O5 2.154(7) .
Cu1 Cu1 2.651(3) 7_565
O1 C20 1.266(8) .
O2 C20 1.263(8) 7_565
O3 C21 1.284(8) 8_576
O4 C21 1.271(8) 2_544
O5 C221 1.04(2) .
O5 C22 1.12(2) .
C1 C2 1.386(9) .
C1 C6 1.425(8) .
C1 C20 1.511(8) .
C2 C3 1.372(9) .
C2 H2 0.9300 .
C3 C4 1.402(9) .
C3 H3 0.9300 .
C4 C5 1.405(9) .
C4 C7 1.506(8) .
C5 C6 1.395(8) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 C12 1.414(9) .
C7 C8 1.419(9) .
C8 C9 1.396(8) .
C8 H8 0.9300 .
C9 C10 1.427(9) .
C9 C14 1.480(9) .
C10 C11 1.393(10) .
C10 H10 0.9300 .
C11 C12 1.409(9) .
C11 C13 1.520(10) .
C12 H12 0.9300 .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
C14 C15 1.377(9) .
C14 C16 1.402(9) .
C15 C19 1.404(9) .
C15 H15 0.9300 .
C16 C17 1.369(9) .
C16 H16 0.9300 .
C17 C18 1.399(9) .
C17 H17 0.9300 .
C18 C19 1.411(9) .
C18 C21 1.524(9) .
C19 H19 0.9300 .
C20 O2 1.263(8) 7_565
C21 O4 1.271(8) 2_564
C21 O3 1.284(8) 8_475
C22 N1 1.41(3) .
C22 H22 0.9300 .
C221 N1 1.36(3) .
C221 H221 0.9300 .
C23 N1 1.470(15) .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C24 N1 1.407(16) .
C24 H24A 0.9600 .
C24 H24B 0.9600 .
C24 H24C 0.9600 .
