#------------------------------------------------------------------------------
#$Date: 2016-02-18 16:37:37 +0100 (jue 18 de feb de 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/45/1514501.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_1514501
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 H24 Cu3 N9 O'
_chemical_formula_weight         621.12
_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                67.952(4)
_cell_angle_beta                 87.743(3)
_cell_angle_gamma                69.803(3)
_cell_formula_units_Z            2
_cell_length_a                   11.3700(4)
_cell_length_b                   11.4274(5)
_cell_length_c                   12.1912(6)
_cell_measurement_reflns_used    5347
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.3873
_cell_measurement_theta_min      2.7674
_cell_volume                     1370.45(12)
_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  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9451
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    2.337
_exptl_absorpt_correction_T_max  0.8535
_exptl_absorpt_correction_T_min  0.6521
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.269
_refine_diff_density_min         -1.093
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         4837
_refine_ls_number_restraints     360
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0570
_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)+(0.1614P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1890
_refine_ls_wR_factor_ref         0.2077
_reflns_number_gt                4031
_reflns_number_total             4837
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc00016h.txt
_cod_data_source_block           Cu-MeCN-100K
_cod_original_cell_volume        1370.45(10)
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               1514501
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
Cu3 Cu 0.68489(4) 0.36753(4) -0.27502(4) 0.02769(12) Uani 1 1 d .
N1 N 1.2778(3) 0.2265(3) 0.9275(3) 0.0338(9) Uani 1 1 d .
C1 C 1.1074(6) 0.5040(5) 0.6507(5) 0.0723(18) Uani 1 1 d U
H1A H 1.0858 0.5855 0.6683 0.108 Uiso 1 1 calc R
H1B H 1.0338 0.5070 0.6090 0.108 Uiso 1 1 calc R
H1C H 1.1769 0.4996 0.6004 0.108 Uiso 1 1 calc R
Cu1 Cu 0.62899(4) -0.18390(4) 0.41948(4) 0.02520(11) Uani 1 1 d .
N2 N 1.2612(3) 0.3385(3) 0.8269(3) 0.0411(10) Uani 1 1 d .
H2 H 1.3170 0.3781 0.8047 0.049 Uiso 1 1 calc R
C2 C 1.1468(4) 0.3816(4) 0.7647(4) 0.0517(11) Uani 1 1 d U
O1 O 0.7020(7) 0.1664(8) 0.1318(7) 0.158(3) Uani 1 1 d .
Cu2 Cu 0.45180(4) 0.12349(4) 0.01006(4) 0.02824(12) Uani 1 1 d .
N3 N 0.8408(3) 0.2273(3) 0.6964(3) 0.0343(8) Uani 1 1 d .
C3 C 1.0866(4) 0.2943(4) 0.8307(4) 0.0476(11) Uani 1 1 d U
C4 C 1.1735(4) 0.1994(4) 0.9312(4) 0.0410(10) Uani 1 1 d U
N4 N 0.6304(3) 0.0901(3) 0.3590(4) 0.0517(11) Uani 1 1 d .
H4 H 0.6092 0.1094 0.2839 0.062 Uiso 1 1 calc R
N5 N 0.6537(3) -0.0318(3) 0.4494(3) 0.0316(8) Uani 1 1 d .
C5 C 1.1573(4) 0.0843(5) 1.0289(4) 0.0501(13) Uani 1 1 d U
H5A H 1.2310 0.0395 1.0882 0.075 Uiso 1 1 calc R
H5B H 1.1486 0.0200 0.9975 0.075 Uiso 1 1 calc R
H5C H 1.0816 0.1165 1.0661 0.075 Uiso 1 1 calc R
N6 N 0.5650(3) -0.0870(3) 0.2528(3) 0.0279(8) Uani 1 1 d .
C6 C 0.9603(4) 0.2992(5) 0.7978(5) 0.0539(11) Uani 1 1 d U
H6A H 0.9094 0.3940 0.7475 0.065 Uiso 1 1 calc R
H6B H 0.9189 0.2732 0.8715 0.065 Uiso 1 1 calc R
N7 N 0.5313(3) 0.2547(3) -0.0843(3) 0.0386(9) Uani 1 1 d .
C7 C 0.9573(4) 0.2122(4) 0.7335(4) 0.0459(10) Uani 1 1 d U
N8 N 0.6735(3) 0.5380(3) -0.3937(3) 0.0364(9) Uani 1 1 d .
C8 C 1.0649(4) 0.1204(4) 0.7141(5) 0.0513(10) Uani 1 1 d U
H8 H 1.1465 0.1119 0.7393 0.062 Uiso 1 1 calc R
C9 C 1.0493(5) 0.0426(5) 0.6574(5) 0.0627(12) Uani 1 1 d U
H9 H 1.1209 -0.0221 0.6438 0.075 Uiso 1 1 calc R
N9 N 0.0873(13) 0.6576(10) -0.1209(10) 0.218(6) Uani 1 1 d .
C10 C 0.9317(4) 0.0577(5) 0.6206(6) 0.0664(11) Uani 1 1 d U
H10 H 0.9209 0.0040 0.5810 0.080 Uiso 1 1 calc R
C11 C 0.8279(4) 0.1516(4) 0.6412(5) 0.0583(10) Uani 1 1 d U
C12 C 0.6914(4) 0.1780(5) 0.6043(6) 0.0686(11) Uani 1 1 d U
H12A H 0.6512 0.1432 0.6769 0.082 Uiso 1 1 calc R
H12B H 0.6463 0.2769 0.5667 0.082 Uiso 1 1 calc R
C13 C 0.6294(6) 0.3201(5) 0.3175(7) 0.103(2) Uani 1 1 d U
H13A H 0.7092 0.3207 0.2842 0.155 Uiso 1 1 calc R
H13B H 0.6049 0.3818 0.3595 0.155 Uiso 1 1 calc R
H13C H 0.5638 0.3496 0.2531 0.155 Uiso 1 1 calc R
C14 C 0.6454(4) 0.1787(4) 0.4036(5) 0.0642(11) Uani 1 1 d U
C15 C 0.6743(4) 0.1164(5) 0.5207(5) 0.0637(11) Uani 1 1 d U
C16 C 0.6794(4) -0.0164(4) 0.5469(5) 0.0523(9) Uani 1 1 d U
C17 C 0.7120(4) -0.1297(5) 0.6638(5) 0.0622(13) Uani 1 1 d U
H17A H 0.6935 -0.2050 0.6580 0.093 Uiso 1 1 calc R
H17B H 0.6623 -0.1004 0.7224 0.093 Uiso 1 1 calc R
H17C H 0.8019 -0.1592 0.6887 0.093 Uiso 1 1 calc R
C18 C 0.5227(3) -0.0144(3) 0.1585(3) 0.0228(8) Uani 1 1 d .
C19 C 0.5890(4) 0.3052(3) -0.1544(4) 0.0359(11) Uani 1 1 d .
C20 C 0.6596(3) 0.6416(4) -0.4671(4) 0.0310(10) Uani 1 1 d .
C21 C 0.215(3) 0.4552(10) 0.0665(10) 0.371(7) Uani 1 1 d U
H21A H 0.3054 0.4366 0.0782 0.557 Uiso 1 1 calc R
H21B H 0.2024 0.3784 0.0576 0.557 Uiso 1 1 calc R
H21C H 0.1749 0.4689 0.1356 0.557 Uiso 1 1 calc R
C22 C 0.158(3) 0.5771(10) -0.0408(10) 0.350(8) Uani 1 1 d U
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
C19 Cu3 N8 136.02(15) . .
C19 Cu3 N3 118.10(14) . 1_554
N8 Cu3 N3 105.80(14) . 1_554
C4 N1 N2 106.5(3) . .
C4 N1 Cu2 134.5(3) . 1_656
N2 N1 Cu2 117.2(3) . 1_656
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 . .
C20 Cu1 N6 136.02(17) 1_546 .
C20 Cu1 N5 125.74(16) 1_546 .
N6 Cu1 N5 98.21(13) . .
N1 N2 C2 111.3(4) . .
N1 N2 H2 124.3 . .
C2 N2 H2 124.3 . .
N2 C2 C3 106.3(4) . .
N2 C2 C1 120.9(5) . .
C3 C2 C1 132.8(5) . .
C18 Cu2 N7 123.70(15) . .
C18 Cu2 N1 135.16(15) . 1_454
N7 Cu2 N1 97.87(14) . 1_454
C18 Cu2 Cu2 69.54(12) . 2_655
N7 Cu2 Cu2 114.26(11) . 2_655
N1 Cu2 Cu2 110.65(11) 1_454 2_655
C11 N3 C7 119.4(4) . .
C11 N3 Cu3 120.6(3) . 1_556
C7 N3 Cu3 120.1(3) . 1_556
C2 C3 C4 105.2(4) . .
C2 C3 C6 126.2(4) . .
C4 C3 C6 128.6(4) . .
N1 C4 C3 110.6(4) . .
N1 C4 C5 121.8(4) . .
C3 C4 C5 127.6(4) . .
N5 N4 C14 109.0(4) . .
N5 N4 H4 125.5 . .
C14 N4 H4 125.5 . .
C16 N5 N4 106.0(3) . .
C16 N5 Cu1 133.5(3) . .
N4 N5 Cu1 120.2(3) . .
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 170.4(3) . .
C3 C6 C7 116.3(4) . .
C3 C6 H6A 108.2 . .
C7 C6 H6A 108.2 . .
C3 C6 H6B 108.2 . .
C7 C6 H6B 108.2 . .
H6A C6 H6B 107.4 . .
C19 N7 Cu2 160.7(4) . .
N3 C7 C8 121.8(5) . .
N3 C7 C6 114.8(4) . .
C8 C7 C6 123.4(4) . .
C20 N8 Cu3 176.0(4) . .
C9 C8 C7 117.8(5) . .
C9 C8 H8 121.1 . .
C7 C8 H8 121.1 . .
C10 C9 C8 120.2(5) . .
C10 C9 H9 119.9 . .
C8 C9 H9 119.9 . .
C9 C10 C11 119.6(5) . .
C9 C10 H10 120.2 . .
C11 C10 H10 120.2 . .
N3 C11 C10 121.2(4) . .
N3 C11 C12 114.2(4) . .
C10 C11 C12 124.6(5) . .
C15 C12 C11 115.3(4) . .
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 . .
C15 C14 N4 109.2(4) . .
C15 C14 C13 132.4(6) . .
N4 C14 C13 118.4(6) . .
C14 C15 C16 104.7(5) . .
C14 C15 C12 126.6(5) . .
C16 C15 C12 128.7(5) . .
N5 C16 C15 111.1(4) . .
N5 C16 C17 121.4(4) . .
C15 C16 C17 127.4(5) . .
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 172.4(3) . .
N7 C19 Cu3 172.0(4) . .
N8 C20 Cu1 176.0(4) . 1_564
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 . .
N9 C22 C21 160(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu3 C19 1.866(4) .
Cu3 N8 1.905(3) .
Cu3 N3 2.059(3) 1_554
N1 C4 1.320(6) .
N1 N2 1.360(4) .
N1 Cu2 1.993(3) 1_656
C1 C2 1.499(7) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
Cu1 C20 1.871(4) 1_546
Cu1 N6 1.938(3) .
Cu1 N5 2.014(3) .
N2 C2 1.365(6) .
N2 H2 0.8800 .
C2 C3 1.392(7) .
Cu2 C18 1.872(3) .
Cu2 N7 1.986(4) .
Cu2 N1 1.993(3) 1_454
Cu2 Cu2 2.7550(9) 2_655
N3 C11 1.325(7) .
N3 C7 1.349(6) .
N3 Cu3 2.059(3) 1_556
C3 C4 1.418(6) .
C3 C6 1.482(7) .
C4 C5 1.468(6) .
N4 N5 1.357(4) .
N4 C14 1.374(7) .
N4 H4 0.8800 .
N5 C16 1.322(6) .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
N6 C18 1.137(4) .
C6 C7 1.489(7) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
N7 C19 1.158(6) .
C7 C8 1.389(6) .
N8 C20 1.146(5) .
C8 C9 1.372(8) .
C8 H8 0.9500 .
C9 C10 1.359(7) .
C9 H9 0.9500 .
N9 C22 1.15(2) .
C10 C11 1.382(7) .
C10 H10 0.9500 .
C11 C12 1.527(7) .
C12 C15 1.489(8) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 C14 1.512(7) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 C15 1.329(8) .
C15 C16 1.409(7) .
C16 C17 1.474(7) .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C20 Cu1 1.871(4) 1_564
C21 C22 1.465(15) .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
