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#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/44/1514498.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_1514498
loop_
_publ_author_name
'Wang, Jun-Hao'
'Li, Mian'
'Li, Dan'
_publ_section_title
;
 A dynamic, luminescent and entangled MOF as a qualitative sensor for
 volatile organic solvents and a quantitative monitor for acetonitrile
 vapour
;
_journal_issue                   4
_journal_name_full               'Chemical Science'
_journal_page_first              1793
_journal_paper_doi               10.1039/c3sc00016h
_journal_volume                  4
_journal_year                    2013
_chemical_formula_sum            'C22 H26 Cu3 N8 O2'
_chemical_formula_weight         625.13
_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                114.171(3)
_cell_angle_beta                 91.497(3)
_cell_angle_gamma                68.347(3)
_cell_formula_units_Z            2
_cell_length_a                   11.5152(3)
_cell_length_b                   11.3120(4)
_cell_length_c                   12.6953(4)
_cell_measurement_reflns_used    6653
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.2907
_cell_measurement_theta_min      3.2223
_cell_volume                     1386.93(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0170
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9785
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    2.312
_exptl_absorpt_correction_T_max  0.7532
_exptl_absorpt_correction_T_min  0.5957
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             634
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.101
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         4889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1364
_reflns_number_gt                4406
_reflns_number_total             4889
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc00016h.txt
_cod_data_source_block           Cu-Ethanol-100K
_cod_original_cell_volume        1386.93(8)
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               1514498
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
Cu1 Cu 1.11949(2) -0.17140(2) -0.40603(2) 0.02137(7) Uani 1 1 d .
N1 N 1.77149(16) 0.23978(18) -0.89787(15) 0.0237(4) Uani 1 1 d .
O1 O 1.1154(3) 0.2545(3) -0.1212(2) 0.1423(9) Uani 1 1 d .
C1 C 1.5916(2) 0.5339(3) -0.6224(2) 0.0461(8) Uani 1 1 d .
H1A H 1.6535 0.5239 -0.5689 0.069 Uiso 1 1 calc R
H1B H 1.5103 0.5467 -0.5878 0.069 Uiso 1 1 calc R
H1C H 1.5814 0.6160 -0.6363 0.069 Uiso 1 1 calc R
Cu2 Cu 0.94181(2) 0.13464(3) 0.00869(2) 0.02270(7) Uani 1 1 d .
N2 N 1.74984(16) 0.35833(19) -0.79804(16) 0.0256(5) Uani 1 1 d .
H2 H 1.8035 0.3997 -0.7771 0.031 Uiso 1 1 calc R
O2 O 0.8383(3) 0.5151(4) 0.0301(3) 0.1310(15) Uani 1 1 d .
C2 C 1.6363(2) 0.4055(2) -0.7345(2) 0.0297(6) Uani 1 1 d .
Cu3 Cu 1.18194(2) 0.36024(2) 0.28921(2) 0.02006(7) Uani 1 1 d .
N3 N 1.34428(15) 0.21531(17) -0.69300(15) 0.0216(4) Uani 1 1 d .
C3 C 1.58182(19) 0.3120(2) -0.7978(2) 0.0292(6) Uani 1 1 d .
N4 N 1.12964(15) 0.10101(17) -0.37094(16) 0.0244(5) Uani 1 1 d .
H4 H 1.1078 0.1328 -0.2955 0.029 Uiso 1 1 calc R
C4 C 1.6688(2) 0.2116(2) -0.8984(2) 0.0273(5) Uani 1 1 d .
N5 N 1.15039(16) -0.03312(18) -0.45053(16) 0.0257(5) Uani 1 1 d .
C5 C 1.6599(2) 0.0861(3) -0.9950(3) 0.0442(8) Uani 1 1 d .
H5A H 1.7356 0.0375 -1.0536 0.066 Uiso 1 1 calc R
H5B H 1.5849 0.1160 -1.0311 0.066 Uiso 1 1 calc R
H5C H 1.6533 0.0221 -0.9640 0.066 Uiso 1 1 calc R
N6 N 1.05413(17) -0.05960(18) -0.24308(15) 0.0252(5) Uani 1 1 d .
C6 C 1.4553(2) 0.3168(2) -0.7642(2) 0.0366(6) Uani 1 1 d .
H6A H 1.4120 0.2982 -0.8340 0.044 Uiso 1 1 calc R
H6B H 1.4039 0.4136 -0.7055 0.044 Uiso 1 1 calc R
N7 N 1.02602(16) 0.25937(19) 0.10563(16) 0.0277(5) Uani 1 1 d .
C7 C 1.45813(19) 0.2148(2) -0.7151(2) 0.0282(6) Uani 1 1 d .
N8 N 1.16389(16) 0.5339(2) 0.41813(17) 0.0299(5) Uani 1 1 d .
C8 C 1.5658(2) 0.1271(3) -0.6927(3) 0.0502(7) Uani 1 1 d .
H8 H 1.6459 0.1263 -0.7101 0.060 Uiso 1 1 calc R
C9 C 1.5564(2) 0.0412(3) -0.6454(3) 0.0628(8) Uani 1 1 d .
H9 H 1.6292 -0.0171 -0.6268 0.075 Uiso 1 1 calc R
C10 C 1.4385(2) 0.0408(3) -0.6249(3) 0.0524(7) Uani 1 1 d .
H10 H 1.4301 -0.0198 -0.5941 0.063 Uiso 1 1 calc R
C11 C 1.3347(2) 0.1287(2) -0.6497(2) 0.0317(6) Uani 1 1 d .
C12 C 1.2022(2) 0.1358(3) -0.6313(2) 0.0406(6) Uani 1 1 d .
H12A H 1.1415 0.2336 -0.6099 0.049 Uiso 1 1 calc R
H12B H 1.1846 0.0746 -0.7062 0.049 Uiso 1 1 calc R
C13 C 1.1320(2) 0.3294(2) -0.3499(3) 0.0433(7) Uani 1 1 d .
H13A H 1.0528 0.3820 -0.2954 0.065 Uiso 1 1 calc R
H13B H 1.1309 0.3729 -0.4028 0.065 Uiso 1 1 calc R
H13C H 1.2032 0.3308 -0.3061 0.065 Uiso 1 1 calc R
C14 C 1.14619(19) 0.1779(2) -0.4203(2) 0.0297(6) Uani 1 1 d .
C15 C 1.1785(2) 0.0924(2) -0.5392(2) 0.0327(6) Uani 1 1 d .
C16 C 1.18092(19) -0.0377(2) -0.55325(19) 0.0280(5) Uani 1 1 d .
C17 C 1.2103(2) -0.1688(3) -0.6636(2) 0.0388(7) Uani 1 1 d .
H17A H 1.3000 -0.2079 -0.6949 0.058 Uiso 1 1 calc R
H17B H 1.1588 -0.1466 -0.7209 0.058 Uiso 1 1 calc R
H17C H 1.1914 -0.2380 -0.6476 0.058 Uiso 1 1 calc R
C18 C 1.01102(19) 0.0070(2) -0.14624(19) 0.0223(5) Uani 1 1 d .
C19 C 1.08652(19) 0.3021(2) 0.17254(18) 0.0217(5) Uani 1 1 d .
C20 C 1.14982(19) 0.6436(2) 0.48843(19) 0.0246(5) Uani 1 1 d .
C21 C 0.6094(6) 0.6266(9) 0.0573(9) 0.215(5) Uani 1 1 d .
H21A H 0.5732 0.5923 0.1021 0.323 Uiso 1 1 calc R
H21B H 0.5461 0.6650 0.0142 0.323 Uiso 1 1 calc R
H21C H 0.6354 0.7007 0.1108 0.323 Uiso 1 1 calc R
C22 C 0.7344(8) 0.4942(6) -0.0361(5) 0.213(3) Uani 1 1 d .
H22A H 0.7317 0.4018 -0.0529 0.255 Uiso 1 1 calc R
H22B H 0.7414 0.5022 -0.1103 0.255 Uiso 1 1 calc R
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
C20 Cu1 N6 134.61(10) 1_544 .
C20 Cu1 N5 123.56(9) 1_544 .
N6 Cu1 N5 101.82(8) . .
C4 N1 N2 105.66(16) . .
C4 N1 Cu2 134.22(14) . 1_654
N2 N1 Cu2 119.22(14) . 1_654
C2 C1 H1A 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C18 Cu2 N1 136.55(8) . 1_456
C18 Cu2 N7 120.64(9) . .
N1 Cu2 N7 98.92(7) 1_456 .
C18 Cu2 Cu2 69.75(7) . 2_755
N1 Cu2 Cu2 113.68(6) 1_456 2_755
N7 Cu2 Cu2 111.80(6) . 2_755
C2 N2 N1 112.28(19) . .
C2 N2 H2 123.9 . .
N1 N2 H2 123.9 . .
N2 C2 C3 105.58(18) . .
N2 C2 C1 122.0(2) . .
C3 C2 C1 132.4(2) . .
C19 Cu3 N8 135.82(8) . .
C19 Cu3 N3 120.51(8) . 1_556
N8 Cu3 N3 103.48(8) . 1_556
C11 N3 C7 119.86(19) . .
C11 N3 Cu3 119.17(14) . 1_554
C7 N3 Cu3 120.75(16) . 1_554
C2 C3 C4 106.3(2) . .
C2 C3 C6 126.70(19) . .
C4 C3 C6 127.0(2) . .
C14 N4 N5 112.40(18) . .
C14 N4 H4 123.8 . .
N5 N4 H4 123.8 . .
N1 C4 C3 110.2(2) . .
N1 C4 C5 120.74(19) . .
C3 C4 C5 129.0(2) . .
C16 N5 N4 104.76(19) . .
C16 N5 Cu1 132.64(16) . .
N4 N5 Cu1 122.34(15) . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C18 N6 Cu1 177.62(19) . .
C3 C6 C7 115.77(19) . .
C3 C6 H6A 108.3 . .
C7 C6 H6A 108.3 . .
C3 C6 H6B 108.3 . .
C7 C6 H6B 108.3 . .
H6A C6 H6B 107.4 . .
C19 N7 Cu2 160.6(2) . .
N3 C7 C8 120.9(2) . .
N3 C7 C6 114.30(19) . .
C8 C7 C6 124.8(2) . .
C20 N8 Cu3 173.7(2) . .
C9 C8 C7 119.6(2) . .
C9 C8 H8 120.2 . .
C7 C8 H8 120.2 . .
C8 C9 C10 118.9(3) . .
C8 C9 H9 120.6 . .
C10 C9 H9 120.6 . .
C11 C10 C9 119.2(3) . .
C11 C10 H10 120.4 . .
C9 C10 H10 120.4 . .
N3 C11 C10 121.4(2) . .
N3 C11 C12 115.2(2) . .
C10 C11 C12 123.4(2) . .
C15 C12 C11 115.3(2) . .
C15 C12 H12A 108.4 . .
C11 C12 H12A 108.4 . .
C15 C12 H12B 108.4 . .
C11 C12 H12B 108.4 . .
H12A C12 H12B 107.5 . .
C14 C13 H13A 109.5 . .
C14 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C14 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
N4 C14 C15 106.7(2) . .
N4 C14 C13 122.4(2) . .
C15 C14 C13 130.8(2) . .
C14 C15 C16 105.4(2) . .
C14 C15 C12 125.9(2) . .
C16 C15 C12 128.7(2) . .
N5 C16 C15 110.7(2) . .
N5 C16 C17 121.0(2) . .
C15 C16 C17 128.3(2) . .
C16 C17 H17A 109.5 . .
C16 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C16 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
N6 C18 Cu2 172.7(2) . .
N7 C19 Cu3 173.7(2) . .
N8 C20 Cu1 175.0(2) . 1_566
C22 C21 H21A 109.5 . .
C22 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C22 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
O2 C22 C21 101.0(5) . .
O2 C22 H22A 111.6 . .
C21 C22 H22A 111.6 . .
O2 C22 H22B 111.6 . .
C21 C22 H22B 111.6 . .
H22A C22 H22B 109.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 C20 1.867(2) 1_544
Cu1 N6 1.9188(17) .
Cu1 N5 2.009(2) .
N1 C4 1.333(3) .
N1 N2 1.358(2) .
N1 Cu2 1.9781(16) 1_654
C1 C2 1.481(3) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
Cu2 C18 1.870(2) .
Cu2 N1 1.9781(16) 1_456
Cu2 N7 1.9928(19) .
Cu2 Cu2 2.7524(5) 2_755
N2 C2 1.354(3) .
N2 H2 0.8800 .
O2 C22 1.480(8) .
C2 C3 1.388(3) .
Cu3 C19 1.867(2) .
Cu3 N8 1.9138(19) .
Cu3 N3 2.0622(17) 1_556
N3 C11 1.341(3) .
N3 C7 1.345(3) .
N3 Cu3 2.0622(17) 1_554
C3 C4 1.401(3) .
C3 C6 1.504(3) .
N4 C14 1.327(3) .
N4 N5 1.367(2) .
N4 H4 0.8800 .
C4 C5 1.484(3) .
N5 C16 1.335(3) .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
N6 C18 1.150(3) .
C6 C7 1.511(4) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
N7 C19 1.150(3) .
C7 C8 1.381(3) .
N8 C20 1.147(3) .
C8 C9 1.370(4) .
C8 H8 0.9500 .
C9 C10 1.391(4) .
C9 H9 0.9500 .
C10 C11 1.370(4) .
C10 H10 0.9500 .
C11 C12 1.517(3) .
C12 C15 1.506(4) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 C14 1.519(3) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 C15 1.385(3) .
C15 C16 1.398(4) .
C16 C17 1.493(3) .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C20 Cu1 1.867(2) 1_566
C21 C22 1.663(9) .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
