#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/45/4324507.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_4324507
loop_
_publ_author_name
'Shenglin Xiang'
'Jing Huang'
'Lei Li'
'Jianyong Zhang'
'Long Jiang'
'Xiaojun Kuang'
'Cheng-Yong Su'
_publ_section_title
;
 Nanotubular Metal-Organic Frameworks with High Porosity Based on T-Shaped
 Pyridyl Dicarboxylate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1743
_journal_page_last               1748
_journal_paper_doi               10.1021/ic102188v
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C17.5 H21.5 Cu N2.5 O7.5'
_chemical_formula_weight         450.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 113.959(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9132(10)
_cell_length_b                   13.5460(11)
_cell_length_c                   13.6700(15)
_cell_measurement_reflns_used    1256
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      62.4743
_cell_measurement_theta_min      3.2602
_cell_volume                     2015.9(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.0855
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0694
_diffrn_reflns_av_sigmaI/netI    0.1127
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5212
_diffrn_reflns_theta_full        62.65
_diffrn_reflns_theta_max         62.65
_diffrn_reflns_theta_min         4.06
_exptl_absorpt_coefficient_mu    1.939
_exptl_absorpt_correction_T_max  0.9093
_exptl_absorpt_correction_T_min  0.8298
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            GREEN
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.491
_refine_diff_density_min         -1.111
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.249
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3121
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.243
_refine_ls_R_factor_all          0.1709
_refine_ls_R_factor_gt           0.1354
_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3586
_refine_ls_wR_factor_ref         0.3736
_reflns_number_gt                1834
_reflns_number_total             3121
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102188v_si_002_1.cif
_cod_data_source_block           1
_cod_original_cell_volume        2015.9(3)
_cod_original_formula_sum        'C17.50 H21.50 Cu N2.50 O7.50'
_cod_database_code               4324507
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.89909(11) 0.05693(11) 0.95938(12) 0.0348(6) Uani 1 1 d . . .
C1 C 0.6285(13) 0.0516(12) 0.8804(13) 0.073(4) Uani 1 1 d . . .
H1A H 0.6501 -0.0162 0.8826 0.088 Uiso 1 1 calc R . .
C2 C 0.5064(12) 0.0772(13) 0.8550(16) 0.084(5) Uani 1 1 d . . .
H2A H 0.4461 0.0270 0.8409 0.101 Uiso 1 1 calc R . .
C3 C 0.4730(11) 0.1754(11) 0.8502(12) 0.064(4) Uani 1 1 d . . .
C4 C 0.5624(12) 0.2426(12) 0.8671(15) 0.082(5) Uani 1 1 d . . .
H4A H 0.5448 0.3112 0.8633 0.098 Uiso 1 1 calc R . .
C5 C 0.6807(12) 0.2095(13) 0.8900(14) 0.078(5) Uani 1 1 d . . .
H5A H 0.7401 0.2590 0.8972 0.094 Uiso 1 1 calc R . .
C6 C 0.3405(10) 0.2021(11) 0.8231(12) 0.057(3) Uani 1 1 d . . .
C7 C 0.2761(10) 0.1452(10) 0.8667(10) 0.051(3) Uani 1 1 d . . .
H7A H 0.3166 0.0931 0.9146 0.061 Uiso 1 1 calc R . .
C8 C 0.1506(9) 0.1640(9) 0.8407(9) 0.044(3) Uani 1 1 d . . .
C9 C 0.0936(9) 0.2371(9) 0.7667(9) 0.045(3) Uani 1 1 d . . .
H9A H 0.0076 0.2463 0.7432 0.054 Uiso 1 1 calc R . .
C10 C 0.1567(9) 0.2962(10) 0.7263(10) 0.048(3) Uani 1 1 d . . .
C11 C 0.2834(10) 0.2788(10) 0.7567(10) 0.052(3) Uani 1 1 d . . .
H11A H 0.3292 0.3208 0.7308 0.063 Uiso 1 1 calc R . .
C12 C 0.0843(9) 0.1012(9) 0.8940(9) 0.042(3) Uani 1 1 d . . .
C13 C 0.0943(10) 0.3752(9) 0.6468(9) 0.045(3) Uani 1 1 d . . .
N1 N 0.7184(8) 0.1225(8) 0.9024(9) 0.052(3) Uani 1 1 d . . .
O1 O 0.1433(7) 0.0309(6) 0.9439(7) 0.050(2) Uani 1 1 d . . .
O2 O -0.0210(6) 0.1289(6) 0.8775(7) 0.048(2) Uani 1 1 d . . .
O3 O -0.0125(6) 0.3555(6) 0.5834(7) 0.049(2) Uani 1 1 d . . .
O4 O 0.1554(7) 0.4491(6) 0.6480(7) 0.053(2) Uani 1 1 d . . .
O5 O 0.482(2) 0.327(2) 0.6146(18) 0.199(10) Uiso 1 1 d D . .
C14 C 0.520(3) 0.242(2) 0.610(3) 0.20(8) Uiso 1 1 d D . .
N2 N 0.637(3) 0.244(2) 0.632(2) 0.22(2) Uiso 1 1 d D . .
C16 C 0.703(4) 0.154(3) 0.631(5) 0.21(5) Uiso 1 1 d D . .
C15 C 0.707(2) 0.336(3) 0.657(5) 0.29(3) Uiso 1 1 d D . .
C19 C -0.099(4) 0.439(4) 0.881(4) 0.078(14) Uiso 0.32 1 d PD . 1
C17 C 0.107(4) 0.394(5) 0.914(4) 0.22(6) Uiso 0.32 1 d PD A 1
C18 C 0.028(5) 0.332(6) 1.036(6) 0.20(5) Uiso 0.32 1 d PD A 1
N3 N 0.015(4) 0.388(3) 0.942(3) 0.13(2) Uiso 0.32 1 d PD A 1
O6 O 0.199(4) 0.346(6) 0.975(6) 0.24(15) Uiso 0.32 1 d PD A 1
C17' C 0.068(3) 0.416(3) 0.933(2) 0.011(9) Uiso 0.18 1 d PD B 2
C19' C -0.096(2) 0.451(3) 0.765(2) 0.012(8) Uiso 0.18 1 d PD B 2
C18' C 0.099(3) 0.549(3) 0.832(3) 0.018(9) Uiso 0.18 1 d PD B 2
O6' O 0.173(4) 0.441(4) 0.995(3) 0.26(17) Uiso 0.18 1 d PD B 2
N3' N 0.025(2) 0.470(2) 0.847(2) 0.15(5) Uiso 0.18 1 d PD B 2
O1W O -0.126(4) 0.388(3) 0.875(4) 0.206(17) Uiso 0.67 1 d P . .
O2W O 0.098(7) 0.488(6) 0.887(6) 0.24(3) Uiso 0.27 1 d P . .
O3W O 0.147(7) 0.380(7) 1.028(6) 0.20(3) Uiso 0.27 1 d P . .
O2'W O 0.108(10) 0.564(9) 0.984(11) 0.23(6) Uiso 0.20 1 d P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 '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
O4 Cu1 O3 166.6(3) 2_646 4_666
O4 Cu1 O1 87.5(4) 2_646 3_657
O3 Cu1 O1 88.9(4) 4_666 3_657
O4 Cu1 O2 91.8(4) 2_646 1_655
O3 Cu1 O2 88.8(4) 4_666 1_655
O1 Cu1 O2 166.7(3) 3_657 1_655
O4 Cu1 N1 93.3(4) 2_646 .
O3 Cu1 N1 99.7(4) 4_666 .
O1 Cu1 N1 90.0(4) 3_657 .
O2 Cu1 N1 103.3(4) 1_655 .
O4 Cu1 Cu1 81.5(2) 2_646 3_757
O3 Cu1 Cu1 85.1(2) 4_666 3_757
O1 Cu1 Cu1 79.0(2) 3_657 3_757
O2 Cu1 Cu1 87.8(2) 1_655 3_757
N1 Cu1 Cu1 167.9(3) . 3_757
N1 C1 C2 121.3(14) . .
N1 C1 H1A 119.3 . .
C2 C1 H1A 119.3 . .
C3 C2 C1 120.2(14) . .
C3 C2 H2A 119.9 . .
C1 C2 H2A 119.9 . .
C4 C3 C2 116.6(13) . .
C4 C3 C6 123.7(14) . .
C2 C3 C6 119.6(13) . .
C3 C4 C5 118.7(15) . .
C3 C4 H4A 120.6 . .
C5 C4 H4A 120.6 . .
N1 C5 C4 127.7(15) . .
N1 C5 H5A 116.1 . .
C4 C5 H5A 116.1 . .
C11 C6 C7 119.8(11) . .
C11 C6 C3 122.2(12) . .
C7 C6 C3 118.0(12) . .
C6 C7 C8 120.5(12) . .
C6 C7 H7A 119.8 . .
C8 C7 H7A 119.8 . .
C9 C8 C7 117.9(11) . .
C9 C8 C12 123.5(9) . .
C7 C8 C12 118.5(10) . .
C10 C9 C8 122.1(10) . .
C10 C9 H9A 118.9 . .
C8 C9 H9A 118.9 . .
C9 C10 C11 118.9(11) . .
C9 C10 C13 121.7(9) . .
C11 C10 C13 119.4(11) . .
C6 C11 C10 120.4(12) . .
C6 C11 H11A 119.8 . .
C10 C11 H11A 119.8 . .
O1 C12 O2 130.7(11) . .
O1 C12 C8 114.2(9) . .
O2 C12 C8 115.1(10) . .
O4 C13 O3 127.9(11) . .
O4 C13 C10 117.1(10) . .
O3 C13 C10 114.9(11) . .
C5 N1 C1 115.1(11) . .
C5 N1 Cu1 133.4(10) . .
C1 N1 Cu1 111.4(9) . .
C12 O1 Cu1 126.6(8) . 3_657
C12 O2 Cu1 115.3(8) . 1_455
C13 O3 Cu1 120.3(8) . 4_465
C13 O4 Cu1 125.0(7) . 2_656
O5 C14 N2 110.7(14) . .
C14 N2 C16 121.0(12) . .
C14 N2 C15 121.3(12) . .
C16 N2 C15 117.8(12) . .
N3 C19 O2'W 81(4) . 3_567
O6 C17 N3 112.5(15) . .
C17 N3 C18 119.9(12) . .
C17 N3 C19 120.6(12) . .
C18 N3 C19 119.5(13) . .
O6' C17' N3' 112.0(14) . .
C17' N3' C18' 120.5(12) . .
C17' N3' C19' 120.0(12) . .
C18' N3' C19' 119.5(12) . .
O2W O2'W C19 140(8) . 3_567
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O4 1.984(8) 2_646
Cu1 O3 1.985(8) 4_666
Cu1 O1 1.990(8) 3_657
Cu1 O2 1.994(8) 1_655
Cu1 N1 2.161(9) .
Cu1 Cu1 2.688(3) 3_757
C1 N1 1.378(19) .
C1 C2 1.39(2) .
C1 H1A 0.9500 .
C2 C3 1.38(2) .
C2 H2A 0.9500 .
C3 C4 1.35(2) .
C3 C6 1.511(17) .
C4 C5 1.39(2) .
C4 H4A 0.9500 .
C5 N1 1.248(19) .
C5 H5A 0.9500 .
C6 C11 1.367(19) .
C6 C7 1.381(18) .
C7 C8 1.413(16) .
C7 H7A 0.9500 .
C8 C9 1.380(17) .
C8 C12 1.532(17) .
C9 C10 1.359(17) .
C9 H9A 0.9500 .
C10 C11 1.413(16) .
C10 C13 1.491(17) .
C11 H11A 0.9500 .
C12 O1 1.215(14) .
C12 O2 1.240(13) .
C13 O4 1.234(15) .
C13 O3 1.243(14) .
O1 Cu1 1.990(8) 3_657
O2 Cu1 1.994(8) 1_455
O3 Cu1 1.985(7) 4_465
O4 Cu1 1.984(8) 2_656
O5 C14 1.252(10) .
C14 N2 1.305(10) .
N2 C16 1.456(10) .
N2 C15 1.459(10) .
C19 N3 1.448(10) .
C19 O2'W 1.89(15) 3_567
C17 O6 1.251(10) .
C17 N3 1.299(10) .
C18 N3 1.447(10) .
C17' O6' 1.246(10) .
C17' N3' 1.300(10) .
C19' N3' 1.450(10) .
C18' N3' 1.450(10) .
O2W O2'W 1.64(12) .
O2'W C19 1.89(15) 3_567
