#------------------------------------------------------------------------------
#$Date: 2017-09-27 15:12:17 +0200 (Wed 27 de Sep de 2017) $
#$Revision: 201370 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/79/7027947.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7027947
loop_
_publ_author_name
'Wang, Xiuli'
'Lin, Hongyan'
'Mu, Bao'
'Tian, Aixiang'
'Liu, Guocheng'
_publ_section_title
;
 Encapsulation of discrete (H2O)12 clusters in a 3D three-fold
 interpenetrating metal--organic framework host with (3,4)-connected
 topology
;
_journal_issue                   27
_journal_name_full               'Dalton Transactions'
_journal_page_first              6187
_journal_page_last               6189
_journal_paper_doi               10.1039/c0dt00302f
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C24 H16 Cu N4 O6, 1.32(H2O)'
_chemical_formula_sum            'C24 H18.64 Cu N4 O7.32'
_chemical_formula_weight         543.97
_chemical_name_systematic        ?
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :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            9
_cell_length_a                   18.5636(3)
_cell_length_b                   18.5636(3)
_cell_length_c                   19.7224(6)
_cell_measurement_reflns_used    8490
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.9136
_cell_measurement_theta_min      2.4230
_cell_volume                     5885.9(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18822
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2299
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0623P)²+9.9813P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1143
_reflns_number_gt                2022
_reflns_number_total             2299
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT00302Fsup1.cif
_cod_data_source_block           complex1
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7027947
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'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+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, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-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+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'
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 0.5000 0.0000 0.5000 0.01766(18) Uani 1 2 d S
N1 N 0.49041(13) 0.00643(13) 0.60119(12) 0.0217(5) Uani 1 1 d .
N2 N 0.49189(14) -0.01349(15) 0.85826(12) 0.0264(5) Uani 1 1 d .
H2A H 0.5168 -0.0386 0.8401 0.032 Uiso 1 1 calc R
C1 C 0.59982(16) 0.15591(15) 0.49146(13) 0.0198(6) Uani 1 1 d .
C2 C 0.63442(16) 0.24783(15) 0.48917(13) 0.0213(6) Uani 1 1 d .
C3 C 0.58116(15) 0.27988(16) 0.48921(13) 0.0208(6) Uani 1 1 d .
H3A H 0.5227 0.2434 0.4893 0.025 Uiso 1 1 calc R
C4 C 0.4328(2) 0.0387(2) 0.69614(15) 0.0368(7) Uani 1 1 d .
H4A H 0.3993 0.0602 0.7128 0.044 Uiso 1 1 calc R
C5 C 0.4449(2) 0.0366(2) 0.62736(14) 0.0343(7) Uani 1 1 d .
H5A H 0.4196 0.0576 0.5974 0.041 Uiso 1 1 calc R
C6 C 0.5258(2) -0.0221(2) 0.64433(15) 0.0385(8) Uani 1 1 d .
H6A H 0.5583 -0.0441 0.6263 0.046 Uiso 1 1 calc R
C7 C 0.5173(2) -0.0213(2) 0.71359(15) 0.0445(9) Uani 1 1 d .
H7A H 0.5441 -0.0416 0.7425 0.053 Uiso 1 1 calc R
C8 C 0.46947(17) 0.00935(17) 0.74073(13) 0.0256(6) Uani 1 1 d .
C9 C 0.45491(19) 0.01485(19) 0.81558(14) 0.0294(7) Uani 1 1 d .
C10 C 0.49397(16) -0.00629(17) 0.92968(15) 0.0248(6) Uani 1 1 d .
C11 C 0.50235(19) -0.06431(19) 0.96734(14) 0.0311(7) Uani 1 1 d .
H11A H 0.5039 -0.1088 0.9450 0.037 Uiso 1 1 calc R
C12 C 0.4915(2) 0.05852(19) 0.96262(14) 0.0321(7) Uani 1 1 d .
H12A H 0.4856 0.0988 0.9372 0.039 Uiso 1 1 calc R
O1 O 0.52031(11) 0.11199(10) 0.49113(9) 0.0210(4) Uani 1 1 d .
O2 O 0.64617(11) 0.12544(11) 0.49497(9) 0.0243(4) Uani 1 1 d .
O3 O 0.41239(17) 0.04415(17) 0.83389(11) 0.0505(7) Uani 1 1 d .
O1W O 0.5201(7) 0.2332(8) 0.8562(8) 0.124(5) Uani 0.33 1 d P
H1WA H 0.5478 0.2459 0.8928 0.149 Uiso 0.33 1 d PR
H1WB H 0.5664 0.2675 0.8381 0.149 Uiso 0.33 1 d PR
O2W O 0.5642(9) 0.2814(8) 0.9999(6) 0.114(4) Uani 0.33 1 d P
H2WA H 0.5562 0.2817 0.9575 0.136 Uiso 0.33 1 d PR
H2WB H 0.6075 0.3293 0.9998 0.136 Uiso 0.33 1 d PR
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'
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
O1 Cu1 O1 180.00(2) 10_656 .
O1 Cu1 N1 90.08(8) 10_656 10_656
O1 Cu1 N1 89.92(8) . 10_656
O1 Cu1 N1 89.92(8) 10_656 .
O1 Cu1 N1 90.08(8) . .
N1 Cu1 N1 180.0 10_656 .
O1 Cu1 C1 150.66(8) 10_656 .
O1 Cu1 C1 29.34(8) . .
N1 Cu1 C1 88.06(8) 10_656 .
N1 Cu1 C1 91.94(8) . .
O1 Cu1 C1 29.34(8) 10_656 10_656
O1 Cu1 C1 150.66(8) . 10_656
N1 Cu1 C1 91.94(8) 10_656 10_656
N1 Cu1 C1 88.06(8) . 10_656
C1 Cu1 C1 180.0 . 10_656
C5 N1 C6 117.5(2) . .
C5 N1 Cu1 120.23(19) . .
C6 N1 Cu1 122.18(19) . .
C9 N2 C10 125.5(2) . .
C9 N2 H2A 117.3 . .
C10 N2 H2A 117.3 . .
O2 C1 O1 123.3(2) . .
O2 C1 C2 121.4(2) . .
O1 C1 C2 115.3(2) . .
O2 C1 Cu1 75.84(14) . .
O1 C1 Cu1 47.48(11) . .
C2 C1 Cu1 162.59(18) . .
C3 C2 C3 120.0(3) . 2_655
C3 C2 C1 119.9(2) . .
C3 C2 C1 120.0(2) 2_655 .
C2 C3 C2 120.0(3) . 3_665
C2 C3 H3A 120.0 . .
C2 C3 H3A 120.0 3_665 .
C5 C4 C8 119.8(3) . .
C5 C4 H4A 120.1 . .
C8 C4 H4A 120.1 . .
N1 C5 C4 122.7(3) . .
N1 C5 H5A 118.7 . .
C4 C5 H5A 118.7 . .
N1 C6 C7 123.1(3) . .
N1 C6 H6A 118.4 . .
C7 C6 H6A 118.4 . .
C6 C7 C8 119.4(3) . .
C6 C7 H7A 120.3 . .
C8 C7 H7A 120.3 . .
C7 C8 C4 117.5(3) . .
C7 C8 C9 125.4(3) . .
C4 C8 C9 117.1(3) . .
O3 C9 N2 124.1(3) . .
O3 C9 C8 119.8(3) . .
N2 C9 C8 116.1(2) . .
C11 C10 C12 119.3(3) . .
C11 C10 N2 118.1(2) . .
C12 C10 N2 122.5(3) . .
C10 C11 C12 120.9(3) . 10_657
C10 C11 H11A 119.6 . .
C12 C11 H11A 119.6 10_657 .
C11 C12 C10 119.8(3) 10_657 .
C11 C12 H12A 120.1 10_657 .
C10 C12 H12A 120.1 . .
C1 O1 Cu1 103.19(15) . .
H1WA O1W H1WB 84.6 . .
H2WA O2W H2WB 94.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.9263(17) 10_656
Cu1 O1 1.9263(17) .
Cu1 N1 2.012(2) 10_656
Cu1 N1 2.013(2) .
Cu1 C1 2.545(2) .
Cu1 C1 2.545(2) 10_656
N1 C5 1.330(4) .
N1 C6 1.336(4) .
N2 C9 1.348(4) .
N2 C10 1.414(4) .
N2 H2A 0.8800 .
C1 O2 1.246(3) .
C1 O1 1.281(3) .
C1 C2 1.493(3) .
C2 C3 1.386(4) .
C2 C3 1.392(4) 2_655
C3 C2 1.392(4) 3_665
C3 H3A 0.9500 .
C4 C5 1.378(4) .
C4 C8 1.380(4) .
C4 H4A 0.9500 .
C5 H5A 0.9500 .
C6 C7 1.376(4) .
C6 H6A 0.9500 .
C7 C8 1.380(4) .
C7 H7A 0.9500 .
C8 C9 1.513(4) .
C9 O3 1.216(3) .
C10 C11 1.380(4) .
C10 C12 1.388(4) .
C11 C12 1.386(4) 10_657
C11 H11A 0.9500 .
C12 C11 1.386(4) 10_657
C12 H12A 0.9500 .
O1W H1WA 0.8499 .
O1W H1WB 0.8499 .
O2W H2WA 0.8501 .
O2W H2WB 0.8499 .
