#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/69/7106986.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_7106986
loop_
_publ_author_name
'Samir Barman'
'Hiroyasu Furukawa'
'Olivier Blacque'
'Koushik Venkatesan'
'Omar M. Yaghi'
'Guo-Xin Jin'
'Heinz Berke'
_publ_section_title
;
 Incorporation of active metal sites in MOFs via in situ generated ligand
 deficient metal-linker complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              11882
_journal_paper_doi               10.1039/c1cc14387e
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C15.71 H21.51 Cu3 N5.90 O13'
_chemical_formula_sum            'C15.71 H21.51 Cu3 N5.9 O13'
_chemical_formula_weight         691.65
_chemical_name_systematic
;
?
;
_space_group_IT_number           142
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   17.6342(6)
_cell_length_b                   17.6342(6)
_cell_length_c                   33.4999(11)
_cell_measurement_reflns_used    2770
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      24.9984
_cell_measurement_theta_min      2.4263
_cell_volume                     10417.3(6)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_molecular_graphics
; ORTEP-3 for Windows, Version 2.01.
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
;
_computing_publication_material
; WinGX -- An integrated system of Windows programs for the solution,
refinment and analysis of single crystal X-ray diffraction data,
Version 1.80.00.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.
SHELXL97. Program for crystal structure refinement.
Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
PLATON for Windows, Version 1.12.
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13.
;
_computing_structure_refinement
; SHELXL97. Program for crystal structure refinement.
Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_solution
; SHELXS97. Program for Crystal Structure solution.
Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
;
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
; Oxford Diffraction (2007). Oxford Diffraction Ltd.,
Xcalibur CCD system
;
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1413
_diffrn_reflns_av_sigmaI/netI    0.1496
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            24570
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.43
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  180
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.499
_exptl_absorpt_correction_T_max  0.788
_exptl_absorpt_correction_T_min  0.604
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5568.8
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.738
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2480
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.737
_refine_ls_R_factor_all          0.1357
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0422P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0930
_reflns_number_gt                978
_reflns_number_total             2480
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc14387e.txt
_cod_data_source_block           MOF-647A
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_original_formula_sum        'C15.71 H21.51 Cu3 N5.90 O13'
_cod_database_code               7106986
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z'
'x, -y, -z+1/2'
'y+1/4, x+3/4, -z+3/4'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1'
'y+3/4, x+5/4, -z+5/4'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z'
'-x, y, z-1/2'
'-y-1/4, -x-3/4, z-3/4'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'-y+1/4, -x-1/4, z-1/4'
'y+1/4, x+1/4, z+1/4'
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
C1 C 0.4622(4) 0.3988(4) 1.05050(15) 0.0436(17) Uani 1 1 d . . .
C2 C 0.4764(4) 0.4081(3) 1.01061(15) 0.0471(18) Uani 1 1 d . . .
H2 H 0.5230 0.4073 0.9976 0.056 Uiso 1 1 calc R . .
C3 C 0.4058(4) 0.4188(3) 0.99434(15) 0.0380(15) Uani 1 1 d . . .
C4 C 0.3774(4) 0.4290(3) 0.95271(16) 0.0428(17) Uani 1 1 d . . .
C5 C 0.5117(4) 0.3885(4) 1.08575(17) 0.0455(18) Uani 1 1 d . . .
N1 N 0.3874(3) 0.4044(3) 1.05787(11) 0.0433(15) Uani 1 1 d . A .
N2 N 0.3516(3) 0.4157(2) 1.02250(12) 0.0371(13) Uani 1 1 d . . .
O1 O 0.2577(3) 0.3628(3) 1.10834(11) 0.0633(13) Uani 1 1 d D A .
H1A H 0.236(3) 0.387(3) 1.0911(14) 0.076 Uiso 1 1 d D . .
H1B H 0.237(3) 0.362(4) 1.1300(9) 0.076 Uiso 1 1 d D . .
O2 O 0.5800(3) 0.3902(2) 1.08274(10) 0.0503(12) Uani 1 1 d . . .
O3A O 0.3665(10) 0.4969(12) 1.1394(5) 0.084(3) Uani 0.451(6) 1 d P A 1
N4 N 0.4181(9) 0.6071(8) 1.1596(4) 0.084(3) Uani 0.451(6) 1 d P A 1
C8 C 0.4159(11) 0.5423(10) 1.1428(5) 0.084(3) Uani 0.451(6) 1 d P A 1
H8 H 0.4614 0.5279 1.1309 0.101 Uiso 0.451(6) 1 calc PR A 1
C9 C 0.3516(10) 0.6358(9) 1.1782(5) 0.084(3) Uani 0.451(6) 1 d P A 1
H9A H 0.3620 0.6849 1.1893 0.126 Uiso 0.451(6) 1 calc PR A 1
H9B H 0.3360 0.6019 1.1990 0.126 Uiso 0.451(6) 1 calc PR A 1
H9C H 0.3118 0.6400 1.1587 0.126 Uiso 0.451(6) 1 calc PR A 1
C10 C 0.4769(9) 0.6528(9) 1.1637(5) 0.084(3) Uani 0.451(6) 1 d P A 1
H10A H 0.4615 0.6978 1.1777 0.126 Uiso 0.451(6) 1 calc PR A 1
H10B H 0.4960 0.6664 1.1379 0.126 Uiso 0.451(6) 1 calc PR A 1
H10C H 0.5160 0.6275 1.1786 0.126 Uiso 0.451(6) 1 calc PR A 1
O3B O 0.3326(6) 0.4899(9) 1.1462(4) 0.084(3) Uani 0.549(6) 1 d PD A 2
H3A H 0.290(2) 0.499(4) 1.139(3) 0.101 Uiso 0.549(6) 1 d PD A 2
H3B H 0.353(5) 0.5231(12) 1.133(2) 0.101 Uiso 0.549(6) 1 d PD A 2
O4 O 0.4763(2) 0.3821(2) 1.11925(11) 0.0530(11) Uani 1 1 d . A .
O5 O 0.4229(2) 0.4283(2) 0.92440(10) 0.0529(13) Uani 1 1 d . . .
O6 O 0.3056(3) 0.4363(2) 0.94993(10) 0.0486(11) Uani 1 1 d . . .
Cu1 Cu 0.36495(5) 0.38031(5) 1.114916(18) 0.0498(3) Uani 1 1 d D . .
Cu2 Cu 0.2500 0.43729(6) 1.0000 0.0393(3) Uani 1 2 d S . .
C6 C 0.2768(9) 0.6050(8) 0.9930(4) 0.069(2) Uani 0.50 1 d P . .
H6 H 0.3074 0.5886 0.9721 0.083 Uiso 0.50 1 calc PR . .
C7A C 0.2236(8) 0.7184(8) 1.0305(4) 0.069(2) Uani 0.50 1 d P . .
H7A1 H 0.2193 0.7715 1.0247 0.104 Uiso 0.50 1 calc PR . .
H7A2 H 0.2468 0.7118 1.0562 0.104 Uiso 0.50 1 calc PR . .
H7A3 H 0.1741 0.6958 1.0306 0.104 Uiso 0.50 1 calc PR . .
C7B C 0.3213(9) 0.7337(8) 0.9795(4) 0.069(2) Uani 0.50 1 d P . .
H7B1 H 0.3034 0.7847 0.9830 0.104 Uiso 0.50 1 calc PR . .
H7B2 H 0.3227 0.7217 0.9516 0.104 Uiso 0.50 1 calc PR . .
H7B3 H 0.3713 0.7291 0.9906 0.104 Uiso 0.50 1 calc PR . .
O7 O 0.2454(8) 0.5590(5) 1.0123(2) 0.069(2) Uani 0.50 1 d P . .
N3 N 0.2707(6) 0.6817(5) 0.9998(5) 0.069(2) Uani 0.50 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 0.0033 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
N1 C1 C2 110.5(5) . .
N1 C1 C5 116.1(5) . .
C2 C1 C5 133.3(6) . .
C1 C2 C3 103.8(6) . .
C1 C2 H2 128.1 . .
C3 C2 H2 128.1 . .
N2 C3 C2 111.2(5) . .
N2 C3 C4 114.9(6) . .
C2 C3 C4 133.8(6) . .
O5 C4 O6 125.9(5) . .
O5 C4 C3 119.7(6) . .
O6 C4 C3 114.4(5) . .
O2 C5 O4 123.8(5) . .
O2 C5 C1 121.2(6) . .
O4 C5 C1 114.9(6) . .
C1 N1 N2 107.9(4) . .
C1 N1 Cu1 110.8(3) . .
N2 N1 Cu1 140.7(4) . .
C3 N2 N1 106.7(5) . .
C3 N2 Cu2 111.6(4) . .
N1 N2 Cu2 141.4(4) . .
Cu1 O1 H1A 118(5) . .
Cu1 O1 H1B 110(5) . .
H1A O1 H1B 115(7) . .
C5 O2 Cu1 111.9(4) . 27_567
C8 O3A Cu1 132.0(15) . .
C8 O3A H3A 136(3) . .
Cu1 O3A H3A 90.4(19) . .
C8 O3A H3B 77(10) . .
Cu1 O3A H3B 129(10) . .
H3A O3A H3B 64(5) . .
C8 N4 C10 128.0(19) . .
C8 N4 C9 119.3(17) . .
C10 N4 C9 112.6(15) . .
O3A C8 N4 132(2) . .
O3A C8 H8 114.1 . .
N4 C8 H8 114.1 . .
N4 C8 H3B 113(2) . .
H8 C8 H3B 127.2 . .
N4 C9 H9A 109.5 . .
N4 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
N4 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
N4 C10 H10A 109.5 . .
N4 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
N4 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
Cu1 O3B H3A 105(2) . .
Cu1 O3B H3B 105(2) . .
H3A O3B H3B 96(2) . .
C5 O4 Cu1 114.8(4) . .
C4 O6 Cu2 116.0(3) . .
O1 Cu1 O2 89.10(17) . 20_658
O1 Cu1 O4 171.3(2) . .
O2 Cu1 O4 89.28(17) 20_658 .
O1 Cu1 N1 96.86(19) . .
O2 Cu1 N1 163.3(2) 20_658 .
O4 Cu1 N1 82.49(19) . .
O1 Cu1 O3A 101.7(5) . .
O2 Cu1 O3A 95.1(5) 20_658 .
O4 Cu1 O3A 86.9(5) . .
N1 Cu1 O3A 98.9(5) . .
O1 Cu1 O3B 86.7(3) . .
O2 Cu1 O3B 87.7(4) 20_658 .
O4 Cu1 O3B 101.7(3) . .
N1 Cu1 O3B 108.1(4) . .
O3A Cu1 O3B 16.6(6) . .
O6 Cu2 O6 179.0(3) 5_557 .
O6 Cu2 N2 82.56(17) 5_557 5_557
O6 Cu2 N2 97.25(17) . 5_557
O6 Cu2 N2 97.25(17) 5_557 .
O6 Cu2 N2 82.56(17) . .
N2 Cu2 N2 157.9(3) 5_557 .
O6 Cu2 O7 80.0(2) 5_557 .
O6 Cu2 O7 101.0(3) . .
N2 Cu2 O7 103.1(4) 5_557 .
N2 Cu2 O7 98.6(4) . .
O6 Cu2 O7 101.0(3) 5_557 5_557
O6 Cu2 O7 80.0(2) . 5_557
N2 Cu2 O7 98.6(4) 5_557 5_557
N2 Cu2 O7 103.1(4) . 5_557
O7 Cu2 O7 22.2(4) . 5_557
O7 C6 N3 123.3(13) . .
O7 C6 H6 118.3 . .
N3 C6 H6 118.3 . .
N3 C7A H7A1 109.5 . .
N3 C7A H7A2 109.5 . .
H7A1 C7A H7A2 109.5 . .
N3 C7A H7A3 109.5 . .
H7A1 C7A H7A3 109.5 . .
H7A2 C7A H7A3 109.5 . .
N3 C7B H7B1 109.5 . .
N3 C7B H7B2 109.5 . .
H7B1 C7B H7B2 109.5 . .
N3 C7B H7B3 109.5 . .
H7B1 C7B H7B3 109.5 . .
H7B2 C7B H7B3 109.5 . .
C6 O7 Cu2 123.7(8) . .
C6 N3 C7B 119.7(13) . .
C6 N3 C7A 126.3(12) . .
C7B N3 C7A 113.4(10) . .
C7B N3 C6 157.4(13) . 5_557
C7A N3 C6 88.3(10) . 5_557
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.346(7) .
C1 C2 1.369(7) .
C1 C5 1.479(8) .
C2 C3 1.372(8) .
C2 H2 0.9300 .
C3 N2 1.344(7) .
C3 C4 1.493(7) .
C4 O5 1.243(7) .
C4 O6 1.276(7) .
C5 O2 1.209(7) .
C5 O4 1.288(6) .
N1 N2 1.358(5) .
N1 Cu1 1.997(4) .
N2 Cu2 1.981(5) .
O1 Cu1 1.928(5) .
O1 H1A 0.81(5) .
O1 H1B 0.81(4) .
O2 Cu1 1.967(3) 27_567
O3A C8 1.19(2) .
O3A Cu1 2.21(2) .
N4 C8 1.275(18) .
N4 C10 1.322(19) .
N4 C9 1.420(19) .
C8 H8 0.9300 .
C8 H3B 1.20(10) .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
O3B Cu1 2.271(15) .
O3B H3A 0.814(10) .
O3B H3B 0.816(10) .
O4 Cu1 1.970(4) .
O6 Cu2 1.943(4) .
Cu1 O2 1.967(3) 20_658
Cu2 O6 1.943(4) 5_557
Cu2 N2 1.981(5) 5_557
Cu2 O7 2.187(8) .
Cu2 O7 2.187(8) 5_557
C6 O7 1.177(14) .
C6 N3 1.377(15) .
C6 H6 0.9300 .
C7A N3 1.471(18) .
C7A H7A1 0.9600 .
C7A H7A2 0.9600 .
C7A H7A3 0.9600 .
C7B N3 1.448(16) .
C7B H7B1 0.9600 .
C7B H7B2 0.9600 .
C7B H7B3 0.9600 .
N3 C6 1.610(15) 5_557
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1A O6 0.81(5) 1.78(5) 2.596(6) 174(7) 5_557
O1 H1B O5 0.81(5) 1.91(2) 2.694(5) 161(6) 12_454
