#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/10/4001076.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_4001076
loop_
_publ_author_name
'Kanoo, Prakash'
'Matsuda, Ryotaro'
'Higuchi, Masakazu'
'Kitagawa, Susumu'
'Maji, Tapas Kumar'
_publ_section_title
;
 New Interpenetrated Copper Coordination Polymer Frameworks having Porous
 Properties
;
_journal_issue                   24
_journal_name_full               'Chemistry of Materials'
_journal_page_first              5860
_journal_paper_doi               10.1021/cm9025683
_journal_volume                  21
_journal_year                    2009
_chemical_formula_sum            'C18 H13 Cu N O4.5'
_chemical_formula_weight         378.83
_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                 113.950(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.094(3)
_cell_length_b                   19.605(3)
_cell_length_c                   11.782(2)
_cell_measurement_temperature    243(2)
_cell_volume                     3608.5(10)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker,2000)'
_computing_data_reduction        'SAINT (Bruker,2000)'
_computing_molecular_graphics    'Mercury 1.4.1'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      243(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0836
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4081
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.27
_exptl_absorpt_coefficient_mu    1.233
_exptl_absorpt_correction_T_max  0.9812
_exptl_absorpt_correction_T_min  0.8678
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   REQABA
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.287
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         4081
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0576
_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)+(0.1021P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1709
_refine_ls_wR_factor_ref         0.1903
_reflns_number_gt                2909
_reflns_number_total             4081
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm9025683_si_002.cif
_cod_data_source_block           compound2
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C18 H13 Cu N O4.50'
_cod_database_code               4001076
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
C1 C 0.5919(2) 0.87057(19) 0.7213(4) 0.0273(8) Uani 1 1 d .
C2 C 0.6421(3) 0.9300(2) 0.7062(4) 0.0316(9) Uani 1 1 d .
C3 C 0.7146(3) 0.9509(2) 0.8043(4) 0.0365(10) Uani 1 1 d .
H1 H 0.7330 0.9271 0.8790 0.044 Uiso 1 1 calc R
C4 C 0.6152(3) 0.9652(2) 0.5924(4) 0.0412(11) Uani 1 1 d .
H2 H 0.5668 0.9503 0.5253 0.049 Uiso 1 1 calc R
C5 C 0.7613(3) 1.0076(2) 0.7939(4) 0.0399(10) Uani 1 1 d .
C6 C 0.6584(3) 1.0201(3) 0.5787(4) 0.0439(11) Uani 1 1 d .
H3 H 0.6385 1.0432 0.5033 0.053 Uiso 1 1 calc R
C7 C 0.7340(3) 1.0430(2) 0.6790(4) 0.0345(9) Uani 1 1 d .
C8 C 0.8358(3) 1.0312(3) 0.8952(5) 0.0553(15) Uani 1 1 d .
H4 H 0.8552 1.0079 0.9704 0.066 Uiso 1 1 calc R
C9 C 0.8788(3) 1.0870(3) 0.8840(4) 0.0513(14) Uani 1 1 d .
H5 H 0.9262 1.1024 0.9522 0.062 Uiso 1 1 calc R
C10 C 0.7809(3) 1.1002(2) 0.6692(4) 0.0360(10) Uani 1 1 d .
H6 H 0.7632 1.1234 0.5941 0.043 Uiso 1 1 calc R
C11 C 0.8523(3) 1.1222(2) 0.7690(4) 0.0368(10) Uani 1 1 d .
C12 C 0.9016(3) 1.1829(2) 0.7585(4) 0.0307(8) Uani 1 1 d .
C13 C 0.6795(4) 0.7349(3) 1.1301(5) 0.0578(16) Uani 1 1 d .
H7 H 0.7001 0.7097 1.0812 0.069 Uiso 1 1 calc R
C14 C 0.5878(4) 0.8135(3) 1.1452(5) 0.0636(17) Uani 1 1 d .
H8 H 0.5422 0.8432 1.1073 0.076 Uiso 1 1 calc R
C15 C 0.7211(5) 0.7301(4) 1.2574(6) 0.092(3) Uani 1 1 d .
H9 H 0.7677 0.7010 1.2935 0.110 Uiso 1 1 calc R
C16 C 0.6278(5) 0.8132(5) 1.2738(5) 0.098(3) Uani 1 1 d .
H10 H 0.6098 0.8431 1.3198 0.117 Uiso 1 1 calc R
C17 C 0.6922(6) 0.7698(5) 1.3317(5) 0.118(4) Uani 1 1 d D
C18 C 0.70144(14) 0.7479(10) 1.4609(7) 0.369(19) Uani 1 1 d D
H11A H 0.6806 0.7017 1.4597 0.443 Uiso 1 1 calc R
H11B H 0.6705 0.7784 1.4928 0.443 Uiso 1 1 calc R
Cu1 Cu 0.54560(3) 0.77681(2) 0.87412(4) 0.02159(19) Uani 1 1 d .
N1 N 0.6108(2) 0.77425(19) 1.0741(3) 0.0347(8) Uani 1 1 d .
O1 O 0.61251(18) 0.84716(15) 0.8291(3) 0.0337(7) Uani 1 1 d .
O2 O 0.53181(18) 0.84880(15) 0.6236(3) 0.0344(7) Uani 1 1 d .
O3 O 0.9571(2) 1.20633(16) 0.8578(3) 0.0372(7) Uani 1 1 d .
O4 O 0.88409(19) 1.20554(16) 0.6499(3) 0.0343(7) Uani 1 1 d .
O5 O 1.0000 1.0622(16) 1.2500 0.49(2) Uiso 1 2 d SD
H12 H 1.0431 1.0886 1.2529 0.071(18) Uiso 1 1 d RD
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 C1 O2 125.9(3) . .
O1 C1 C2 117.6(3) . .
O2 C1 C2 116.5(3) . .
C3 C2 C4 119.5(4) . .
C3 C2 C1 119.8(4) . .
C4 C2 C1 120.8(4) . .
C2 C3 C5 121.0(4) . .
C6 C4 C2 121.3(4) . .
C3 C5 C7 119.4(4) . .
C3 C5 C8 122.1(4) . .
C7 C5 C8 118.5(4) . .
C4 C6 C7 120.5(4) . .
C10 C7 C5 119.2(4) . .
C10 C7 C6 122.5(4) . .
C5 C7 C6 118.3(4) . .
C9 C8 C5 121.2(4) . .
C8 C9 C11 120.6(4) . .
C11 C10 C7 121.1(4) . .
C10 C11 C9 119.4(4) . .
C10 C11 C12 121.0(4) . .
C9 C11 C12 119.6(4) . .
O3 C12 O4 126.2(4) . .
O3 C12 C11 116.9(4) . .
O4 C12 C11 116.8(4) . .
N1 C13 C15 122.7(5) . .
N1 C14 C16 123.6(5) . .
C13 C15 C17 118.9(5) . .
C17 C16 C14 119.9(6) . .
C16 C17 C15 117.4(5) . .
C16 C17 C18 114.7(8) . .
C15 C17 C18 123.0(9) . .
C17 C18 C18 103.3(8) . 7_668
O4 Cu1 O2 173.06(12) 4_646 2_656
O4 Cu1 O1 90.18(14) 4_646 .
O2 Cu1 O1 88.20(14) 2_656 .
O4 Cu1 O3 88.73(15) 4_646 3_445
O2 Cu1 O3 90.59(15) 2_656 3_445
O1 Cu1 O3 160.87(13) . 3_445
O4 Cu1 N1 93.80(13) 4_646 .
O2 Cu1 N1 93.13(13) 2_656 .
O1 Cu1 N1 102.00(13) . .
O3 Cu1 N1 97.13(14) 3_445 .
O4 Cu1 Cu1 87.79(9) 4_646 2_656
O2 Cu1 Cu1 85.30(9) 2_656 2_656
O1 Cu1 Cu1 81.57(8) . 2_656
O3 Cu1 Cu1 79.30(9) 3_445 2_656
N1 Cu1 Cu1 176.07(11) . 2_656
C14 N1 C13 117.1(4) . .
C14 N1 Cu1 121.8(3) . .
C13 N1 Cu1 120.9(3) . .
C1 O1 Cu1 124.3(2) . .
C1 O2 Cu1 122.5(3) . 2_656
C12 O3 Cu1 126.7(3) . 3
C12 O4 Cu1 119.5(3) . 4_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.259(5) .
C1 O2 1.266(5) .
C1 C2 1.501(5) .
C2 C3 1.369(6) .
C2 C4 1.408(6) .
C3 C5 1.403(6) .
C4 C6 1.351(6) .
C5 C7 1.422(6) .
C5 C8 1.422(6) .
C6 C7 1.424(6) .
C7 C10 1.410(5) .
C8 C9 1.355(6) .
C9 C11 1.422(6) .
C10 C11 1.376(6) .
C11 C12 1.493(5) .
C12 O3 1.256(5) .
C12 O4 1.270(5) .
C13 N1 1.333(6) .
C13 C15 1.378(8) .
C14 N1 1.310(6) .
C14 C16 1.387(8) .
C15 C17 1.403(10) .
C16 C17 1.339(10) .
C17 C18 1.528(8) .
C18 C18 1.5395(11) 7_668
Cu1 O4 1.937(3) 4_646
Cu1 O2 1.942(3) 2_656
Cu1 O1 1.996(3) .
Cu1 O3 2.000(3) 3_445
Cu1 N1 2.160(4) .
Cu1 Cu1 2.6986(9) 2_656
O2 Cu1 1.942(3) 2_656
O3 Cu1 2.000(3) 3
O4 Cu1 1.937(3) 4_656
