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#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/72/7117296.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_7117296
loop_
_publ_author_name
'Chao Huang'
'Jie Wu'
'Chuanjun Song'
'Ran Ding'
'Yan Qiao'
'Hongwei Hou'
'Junbiao Chang'
'Yaoting Fan'
_publ_section_title
;
 Reversible conversion of valence-tautomeric copper metal-organic
 frameworks dependent single-crystal-to-single-crystal
 oxidation/reduction: a redox-switchable catalyst for C-H bonds activation
 reaction
;
_journal_name_full               Chem.Commun.
_journal_page_first              10353
_journal_paper_doi               10.1039/C5cc02432C
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C6 H7 Cu2 N9 O2.50'
_chemical_formula_sum            'C6 H7 Cu2 N9 O2.5'
_chemical_formula_weight         372.29
_chemical_name_systematic        'Cu(I) complex'
_chemical_properties_physical
'Air-sensitive, Heat-sensitive, Oxygen-sensitive'
_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
_audit_update_record
;
2015-01-03 deposited with the CCDC.
2015-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 118.79(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.258(5)
_cell_length_b                   9.4877(19)
_cell_length_c                   16.473(3)
_cell_measurement_reflns_used    5358
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.9043
_cell_measurement_theta_min      1.9157
_cell_volume                     3322.7(15)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  Saturn724
_diffrn_measurement_method       dtprofit.ref
_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  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12534
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.35
_diffrn_standards_number         4190
_exptl_absorpt_coefficient_mu    2.574
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8205
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrystalClear (Rigaku/MSC Inc., 2006)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.172
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3087
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0934P)²+18.3884P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1665
_refine_ls_wR_factor_ref         0.1689
_reflns_number_gt                2881
_reflns_number_total             3087
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc02432c2.cif
_cod_data_source_block           a
_cod_original_cell_volume        3322.7(12)
_cod_original_sg_symbol_Hall     '-C 2yc  '
_cod_original_sg_symbol_H-M      'C2/c  '
_cod_original_formula_sum        'C6 H7 Cu2 N9 O2.50'
_cod_database_code               7117296
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.04272(3) 0.17662(6) 0.03882(4) 0.0242(2) Uani 1 1 d . . .
Cu2 Cu 0.04255(3) 0.38483(6) 0.37785(4) 0.0251(2) Uani 1 1 d . . .
O1 O 0.2311(7) 0.8759(16) 0.6898(11) 0.195(5) Uani 1 1 d U . .
O2 O 0.3816(13) 0.916(3) 0.8489(19) 0.329(12) Uani 1 1 d U . .
N1 N 0.13703(19) 0.0186(5) 0.5300(3) 0.0303(10) Uani 1 1 d . . .
N2 N 0.07927(18) 0.0066(5) 0.5216(3) 0.0257(9) Uani 1 1 d . . .
N3 N 0.04633(18) 0.1198(4) 0.4829(3) 0.0219(9) Uani 1 1 d . . .
N4 N 0.08149(18) 0.2100(4) 0.4640(3) 0.0233(8) Uani 1 1 d . . .
N5 N 0.08264(18) 0.3183(4) 0.2988(3) 0.0222(9) Uani 1 1 d . . .
N6 N 0.04816(18) 0.3015(5) 0.2069(3) 0.0229(9) Uani 1 1 d . . .
N7 N 0.08206(19) 0.2366(5) 0.1764(3) 0.0261(9) Uani 1 1 d . . .
N8 N 0.13992(18) 0.2109(5) 0.2476(3) 0.0274(9) Uani 1 1 d . . .
N9 N 0.0440(2) 0.4345(6) -0.0712(4) 0.0458(13) Uani 1 1 d . . .
C1 C 0.2509(2) 0.3028(6) 0.4230(3) 0.0249(11) Uani 1 1 d . . .
H1 H 0.2514 0.3390 0.3709 0.030 Uiso 1 1 calc R . .
C2 C 0.1937(2) 0.2566(5) 0.4147(3) 0.0228(10) Uani 1 1 d . . .
C3 C 0.1928(2) 0.2031(5) 0.4938(3) 0.0235(10) Uani 1 1 d . . .
C4 C 0.1367(2) 0.1450(5) 0.4934(3) 0.0219(10) Uani 1 1 d . . .
C5 C 0.1379(2) 0.2608(5) 0.3216(3) 0.0222(10) Uani 1 1 d . . .
C6 C 0.0436(3) 0.3319(5) -0.0363(4) 0.0265(11) Uani 1 1 d . . .
O3 O 0.412(2) 0.687(5) 0.736(3) 0.33(2) Uani 0.50 1 d PU . .
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
C6 Cu1 N2 115.0(2) . 6
C6 Cu1 N7 110.5(2) . .
N2 Cu1 N7 112.70(17) 6 .
C6 Cu1 N3 114.7(2) . 2
N2 Cu1 N3 103.94(16) 6 2
N7 Cu1 N3 98.79(16) . 2
N9 Cu2 N5 129.8(2) 6_566 .
N9 Cu2 N4 120.7(2) 6_566 .
N5 Cu2 N4 89.40(16) . .
N9 Cu2 N6 114.9(2) 6_566 2
N5 Cu2 N6 97.23(16) . 2
N4 Cu2 N6 97.95(16) . 2
C4 N1 N2 104.4(4) . .
N3 N2 N1 110.0(4) . .
N3 N2 Cu1 124.4(3) . 6_556
N1 N2 Cu1 124.2(3) . 6_556
N2 N3 N4 109.1(4) . .
N2 N3 Cu1 129.5(3) . 2
N4 N3 Cu1 121.1(3) . 2
C4 N4 N3 105.0(4) . .
C4 N4 Cu2 131.2(3) . .
N3 N4 Cu2 122.1(3) . .
C5 N5 N6 105.5(4) . .
C5 N5 Cu2 131.9(3) . .
N6 N5 Cu2 121.4(3) . .
N7 N6 N5 109.0(4) . .
N7 N6 Cu2 124.8(3) . 2
N5 N6 Cu2 126.0(3) . 2
N6 N7 N8 109.5(4) . .
N6 N7 Cu1 120.5(3) . .
N8 N7 Cu1 129.9(3) . .
C5 N8 N7 104.6(4) . .
C6 N9 Cu2 174.6(5) . 6_565
C3 C1 C2 122.7(4) 7_556 .
C3 C1 H1 118.7 7_556 .
C2 C1 H1 118.7 . .
C1 C2 C3 118.6(4) . .
C1 C2 C5 117.5(4) . .
C3 C2 C5 123.8(4) . .
C1 C3 C2 118.7(4) 7_556 .
C1 C3 C4 117.2(4) 7_556 .
C2 C3 C4 124.0(4) . .
N1 C4 N4 111.4(4) . .
N1 C4 C3 122.0(4) . .
N4 C4 C3 126.5(5) . .
N5 C5 N8 111.5(4) . .
N5 C5 C2 126.9(4) . .
N8 C5 C2 121.5(4) . .
N9 C6 Cu1 170.5(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 C6 1.930(5) .
Cu1 N2 2.032(4) 6
Cu1 N7 2.070(4) .
Cu1 N3 2.083(4) 2
Cu2 N9 1.902(6) 6_566
Cu2 N5 2.064(4) .
Cu2 N4 2.090(4) .
Cu2 N6 2.111(4) 2
N1 C4 1.340(7) .
N1 N2 1.345(6) .
N2 N3 1.307(6) .
N2 Cu1 2.032(4) 6_556
N3 N4 1.346(6) .
N3 Cu1 2.083(4) 2
N4 C4 1.335(6) .
N5 C5 1.324(6) .
N5 N6 1.340(6) .
N6 N7 1.307(6) .
N6 Cu2 2.111(4) 2
N7 N8 1.350(6) .
N8 C5 1.329(6) .
N9 C6 1.133(8) .
N9 Cu2 1.902(6) 6_565
C1 C3 1.395(7) 7_556
C1 C2 1.397(6) .
C1 H1 0.9300 .
C2 C3 1.407(7) .
C2 C5 1.478(6) .
C3 C1 1.395(7) 7_556
C3 C4 1.466(6) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
C4 N1 N2 N3 -0.6(6) . . . .
C4 N1 N2 Cu1 166.5(3) . . . 6_556
N1 N2 N3 N4 0.5(6) . . . .
Cu1 N2 N3 N4 -166.6(3) 6_556 . . .
N1 N2 N3 Cu1 -173.8(3) . . . 2
Cu1 N2 N3 Cu1 19.1(6) 6_556 . . 2
N2 N3 N4 C4 -0.2(5) . . . .
Cu1 N3 N4 C4 174.7(3) 2 . . .
N2 N3 N4 Cu2 166.9(3) . . . .
Cu1 N3 N4 Cu2 -18.2(5) 2 . . .
N9 Cu2 N4 C4 -100.5(5) 6_566 . . .
N5 Cu2 N4 C4 37.0(5) . . . .
N6 Cu2 N4 C4 134.2(4) 2 . . .
N9 Cu2 N4 N3 96.2(4) 6_566 . . .
N5 Cu2 N4 N3 -126.3(4) . . . .
N6 Cu2 N4 N3 -29.1(4) 2 . . .
N9 Cu2 N5 C5 91.9(5) 6_566 . . .
N4 Cu2 N5 C5 -39.1(5) . . . .
N6 Cu2 N5 C5 -137.0(4) 2 . . .
N9 Cu2 N5 N6 -102.4(4) 6_566 . . .
N4 Cu2 N5 N6 126.7(4) . . . .
N6 Cu2 N5 N6 28.8(3) 2 . . .
C5 N5 N6 N7 -0.2(5) . . . .
Cu2 N5 N6 N7 -169.3(3) . . . .
C5 N5 N6 Cu2 -174.1(3) . . . 2
Cu2 N5 N6 Cu2 16.8(5) . . . 2
N5 N6 N7 N8 -0.7(6) . . . .
Cu2 N6 N7 N8 173.2(3) 2 . . .
N5 N6 N7 Cu1 175.0(3) . . . .
Cu2 N6 N7 Cu1 -11.1(6) 2 . . .
C6 Cu1 N7 N6 83.8(4) . . . .
N2 Cu1 N7 N6 -146.0(4) 6 . . .
N3 Cu1 N7 N6 -36.8(4) 2 . . .
C6 Cu1 N7 N8 -101.5(5) . . . .
N2 Cu1 N7 N8 28.7(5) 6 . . .
N3 Cu1 N7 N8 137.9(5) 2 . . .
N6 N7 N8 C5 1.4(6) . . . .
Cu1 N7 N8 C5 -173.8(4) . . . .
C3 C1 C2 C3 0.6(9) 7_556 . . .
C3 C1 C2 C5 -176.6(5) 7_556 . . .
C1 C2 C3 C1 -0.6(8) . . . 7_556
C5 C2 C3 C1 176.4(5) . . . 7_556
C1 C2 C3 C4 -176.9(5) . . . .
C5 C2 C3 C4 0.1(8) . . . .
N2 N1 C4 N4 0.5(6) . . . .
N2 N1 C4 C3 176.4(5) . . . .
N3 N4 C4 N1 -0.2(5) . . . .
Cu2 N4 C4 N1 -165.7(4) . . . .
N3 N4 C4 C3 -175.9(5) . . . .
Cu2 N4 C4 C3 18.7(8) . . . .
C1 C3 C4 N1 -47.3(7) 7_556 . . .
C2 C3 C4 N1 129.0(6) . . . .
C1 C3 C4 N4 128.0(5) 7_556 . . .
C2 C3 C4 N4 -55.7(8) . . . .
N6 N5 C5 N8 1.1(6) . . . .
Cu2 N5 C5 N8 168.6(3) . . . .
N6 N5 C5 C2 177.5(5) . . . .
Cu2 N5 C5 C2 -15.1(8) . . . .
N7 N8 C5 N5 -1.6(6) . . . .
N7 N8 C5 C2 -178.1(4) . . . .
C1 C2 C5 N5 -128.7(6) . . . .
C3 C2 C5 N5 54.3(8) . . . .
C1 C2 C5 N8 47.3(7) . . . .
C3 C2 C5 N8 -129.7(6) . . . .
Cu2 N9 C6 Cu1 -14(9) 6_565 . . .
N2 Cu1 C6 N9 -155(3) 6 . . .
N7 Cu1 C6 N9 -26(3) . . . .
N3 Cu1 C6 N9 84(3) 2 . . .
