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#$Date: 2016-02-18 16:37:37 +0100 (jue 18 de feb de 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/47/1514756.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_1514756
loop_
_publ_author_name
'Li, Jia'
'Huang, Peng'
'Wu, Xue-Ru'
'Tao, Jun'
'Huang, Rong-Bin'
'Zheng, Lan-Sun'
_publ_section_title
;
 Metal-organic frameworks displaying single crystal-to-single crystal
 transformation through postsynthetic uptake of metal clusters
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              3232
_journal_paper_doi               10.1039/c3sc51379c
_journal_volume                  4
_journal_year                    2013
_chemical_formula_sum            'C78 H106 Co3 N8 O31'
_chemical_formula_weight         1828.50
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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            4
_cell_length_a                   17.446(4)
_cell_length_b                   27.758(6)
_cell_length_c                   18.762(4)
_cell_measurement_temperature    173(2)
_cell_volume                     9086(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1010
_diffrn_reflns_av_sigmaI/netI    0.0764
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            77211
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.21
_exptl_absorpt_coefficient_mu    0.623
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3836
_refine_diff_density_max         1.332
_refine_diff_density_min         -1.106
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         10594
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1485
_refine_ls_R_factor_gt           0.0917
_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)+(0.1625P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2542
_refine_ls_wR_factor_ref         0.2809
_reflns_number_gt                5999
_reflns_number_total             10594
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc51379c.txt
_cod_data_source_block           1c
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               1514756
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
Co1 Co 0.49344(3) 0.31713(2) 0.03322(4) 0.0634(3) Uani 1 1 d .
Co2 Co 0.38134(3) 0.2500 0.14526(5) 0.0504(3) Uani 1 2 d S
O1W O 0.4768(3) 0.2995(3) -0.0763(3) 0.154(2) Uani 1 1 d .
O7 O 0.4745(2) 0.2500 0.0723(3) 0.0687(12) Uani 1 2 d S
O1 O 0.56047(17) 0.38127(16) -0.0041(3) 0.1214(18) Uani 1 1 d .
O2 O 0.61509(17) 0.31294(13) 0.0199(2) 0.0836(11) Uani 1 1 d .
O3 O 1.31656(14) 0.30131(11) 0.09230(19) 0.0689(9) Uani 1 1 d .
O4 O 1.39021(17) 0.34866(18) 0.0279(3) 0.152(3) Uani 1 1 d .
O5 O 1.06916(16) 0.69600(10) -0.29303(18) 0.0657(8) Uani 1 1 d .
O6 O 0.9868(2) 0.65979(16) -0.3646(3) 0.1167(17) Uani 1 1 d .
C1 C 0.6189(2) 0.3553(2) 0.0008(3) 0.0791(15) Uani 1 1 d .
C2 C 0.6962(2) 0.37792(17) -0.0138(3) 0.0726(14) Uani 1 1 d .
C3 C 0.7606(3) 0.3497(2) -0.0125(4) 0.115(3) Uani 1 1 d .
H3A H 0.7570 0.3172 -0.0007 0.138 Uiso 1 1 calc R
C4 C 0.8314(3) 0.3698(2) -0.0290(4) 0.122(3) Uani 1 1 d .
H4A H 0.8743 0.3500 -0.0296 0.146 Uiso 1 1 calc R
C5 C 0.8401(2) 0.41721(17) -0.0440(3) 0.0755(15) Uani 1 1 d .
C6 C 0.7766(2) 0.4456(2) -0.0421(4) 0.102(2) Uani 1 1 d .
H6A H 0.7811 0.4785 -0.0511 0.123 Uiso 1 1 calc R
C7 C 0.7047(3) 0.4260(2) -0.0268(4) 0.105(2) Uani 1 1 d .
H7A H 0.6620 0.4460 -0.0255 0.126 Uiso 1 1 calc R
C8 C 1.3266(2) 0.33492(18) 0.0514(3) 0.0756(15) Uani 1 1 d .
C9 C 1.2579(2) 0.36442(17) 0.0282(3) 0.0719(14) Uani 1 1 d .
C10 C 1.2621(2) 0.3976(2) -0.0247(4) 0.106(2) Uani 1 1 d .
H10A H 1.3096 0.4048 -0.0446 0.127 Uiso 1 1 calc R
C11 C 1.1973(3) 0.4210(2) -0.0498(4) 0.096(2) Uani 1 1 d .
H11A H 1.2014 0.4418 -0.0884 0.115 Uiso 1 1 calc R
C12 C 1.1268(2) 0.41379(18) -0.0182(3) 0.0779(16) Uani 1 1 d .
C13 C 1.1238(2) 0.38317(18) 0.0404(3) 0.0801(17) Uani 1 1 d .
H13A H 1.0781 0.3796 0.0653 0.096 Uiso 1 1 calc R
C14 C 1.1877(2) 0.35818(17) 0.0619(3) 0.0774(15) Uani 1 1 d .
H14A H 1.1839 0.3367 0.0997 0.093 Uiso 1 1 calc R
C15 C 1.0247(2) 0.66265(17) -0.3083(3) 0.0696(13) Uani 1 1 d .
C16 C 1.0153(2) 0.62250(15) -0.2567(3) 0.0675(14) Uani 1 1 d .
C17 C 0.9612(2) 0.58520(17) -0.2700(3) 0.0823(16) Uani 1 1 d .
H17A H 0.9302 0.5867 -0.3102 0.099 Uiso 1 1 calc R
C18 C 0.9547(2) 0.54744(18) -0.2244(3) 0.0841(17) Uani 1 1 d .
H18A H 0.9179 0.5240 -0.2335 0.101 Uiso 1 1 calc R
C19 C 1.00069(19) 0.54276(17) -0.1651(3) 0.0709(15) Uani 1 1 d .
C20 C 1.0543(2) 0.57949(17) -0.1516(3) 0.0739(14) Uani 1 1 d .
H20A H 1.0864 0.5772 -0.1122 0.089 Uiso 1 1 calc R
C21 C 1.0599(2) 0.61872(15) -0.1958(3) 0.0642(12) Uani 1 1 d .
H21A H 1.0942 0.6432 -0.1847 0.077 Uiso 1 1 calc R
C22 C 0.9174(2) 0.43872(17) -0.0601(3) 0.0719(14) Uani 1 1 d .
C23 C 0.9832(2) 0.41688(17) -0.0348(3) 0.0730(15) Uani 1 1 d .
H23A H 0.9795 0.3881 -0.0096 0.088 Uiso 1 1 calc R
C24 C 1.0564(2) 0.43786(18) -0.0469(3) 0.0756(15) Uani 1 1 d .
C25 C 1.0606(2) 0.47863(16) -0.0884(3) 0.0792(16) Uani 1 1 d .
H25A H 1.1083 0.4923 -0.0973 0.095 Uiso 1 1 calc R
C26 C 0.9951(2) 0.50010(15) -0.1178(3) 0.0705(14) Uani 1 1 d .
C27 C 0.9239(2) 0.47932(16) -0.1023(3) 0.0781(16) Uani 1 1 d .
H27A H 0.8797 0.4932 -0.1209 0.094 Uiso 1 1 calc R
O8 O 0.2936(3) 0.2500 0.2240(3) 0.0873(16) Uani 1 2 d SD
N1 N 0.1605(7) 0.2500 0.2457(11) 0.344(17) Uani 1 2 d SD
C28 C 0.2258(5) 0.2500 0.2027(8) 0.38(2) Uani 1 2 d SD
H28A H 0.2181 0.2500 0.1537 0.460 Uiso 1 2 calc SR
C29 C 0.1764(15) 0.2500 0.3291(9) 0.280(16) Uani 1 2 d SD
C30 C 0.0832(11) 0.2500 0.1994(13) 0.38(2) Uani 1 2 d SD
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'
Co Co 0.3494 0.9721 '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 Co1 O7 105.84(16) 1_455 .
O4 Co1 O6 93.5(2) 1_455 2_665
O7 Co1 O6 88.63(19) . 2_665
O4 Co1 O1W 86.0(3) 1_455 .
O7 Co1 O1W 96.6(2) . .
O6 Co1 O1W 174.7(2) 2_665 .
O4 Co1 O2 155.32(15) 1_455 .
O7 Co1 O2 98.83(15) . .
O6 Co1 O2 87.68(17) 2_665 .
O1W Co1 O2 90.6(2) . .
O4 Co1 O1 96.09(14) 1_455 .
O7 Co1 O1 157.92(14) . .
O6 Co1 O1 87.52(19) 2_665 .
O1W Co1 O1 87.3(2) . .
O2 Co1 O1 59.30(13) . .
O4 Co1 C1 125.98(17) 1_455 .
O7 Co1 C1 128.16(17) . .
O6 Co1 C1 87.00(17) 2_665 .
O1W Co1 C1 89.0(2) . .
O2 Co1 C1 29.40(14) . .
O1 Co1 C1 29.90(15) . .
O3 Co2 O3 86.84(18) 7_465 1_455
O3 Co2 O5 171.12(12) 7_465 2_665
O3 Co2 O5 89.89(13) 1_455 2_665
O3 Co2 O5 89.89(13) 7_465 8_756
O3 Co2 O5 171.12(12) 1_455 8_756
O5 Co2 O5 92.13(18) 2_665 8_756
O3 Co2 O7 96.23(13) 7_465 .
O3 Co2 O7 96.23(13) 1_455 .
O5 Co2 O7 92.34(12) 2_665 .
O5 Co2 O7 92.34(12) 8_756 .
O3 Co2 O8 86.59(14) 7_465 .
O3 Co2 O8 86.59(14) 1_455 .
O5 Co2 O8 84.97(14) 2_665 .
O5 Co2 O8 84.97(14) 8_756 .
O7 Co2 O8 176.1(2) . .
Co1 O7 Co1 133.3(2) . 7_565
Co1 O7 Co2 110.92(11) . .
Co1 O7 Co2 110.92(11) 7_565 .
C1 O1 Co1 86.8(3) . .
C1 O2 Co1 92.0(3) . .
C8 O3 Co2 138.4(3) . 1_655
C8 O4 Co1 130.1(3) . 1_655
C15 O5 Co2 131.9(3) . 2_664
C15 O6 Co1 133.0(3) . 2_664
O2 C1 O1 121.9(4) . .
O2 C1 C2 119.8(4) . .
O1 C1 C2 118.3(5) . .
O2 C1 Co1 58.6(2) . .
O1 C1 Co1 63.3(2) . .
C2 C1 Co1 176.3(4) . .
C7 C2 C3 118.2(4) . .
C7 C2 C1 122.3(4) . .
C3 C2 C1 119.4(4) . .
C2 C3 C4 119.7(5) . .
C5 C4 C3 122.4(5) . .
C4 C5 C6 117.8(4) . .
C4 C5 C22 121.9(4) . .
C6 C5 C22 120.3(4) . .
C5 C6 C7 120.7(5) . .
C2 C7 C6 121.0(5) . .
O3 C8 O4 125.6(4) . .
O3 C8 C9 118.6(4) . .
O4 C8 C9 115.8(4) . .
C10 C9 C14 117.7(4) . .
C10 C9 C8 122.3(4) . .
C14 C9 C8 120.0(4) . .
C9 C10 C11 121.5(4) . .
C12 C11 C10 120.9(5) . .
C11 C12 C13 117.4(4) . .
C11 C12 C24 120.8(4) . .
C13 C12 C24 121.8(4) . .
C14 C13 C12 120.7(4) . .
C13 C14 C9 121.3(4) . .
O5 C15 O6 125.0(5) . .
O5 C15 C16 118.5(5) . .
O6 C15 C16 116.4(4) . .
C21 C16 C17 117.5(4) . .
C21 C16 C15 122.2(4) . .
C17 C16 C15 120.3(5) . .
C18 C17 C16 120.5(5) . .
C17 C18 C19 122.1(4) . .
C18 C19 C20 117.7(4) . .
C18 C19 C26 121.3(4) . .
C20 C19 C26 121.0(5) . .
C21 C20 C19 120.9(4) . .
C20 C21 C16 121.2(4) . .
C27 C22 C23 119.1(4) . .
C27 C22 C5 120.8(4) . .
C23 C22 C5 120.0(4) . .
C22 C23 C24 120.8(4) . .
C25 C24 C23 118.3(4) . .
C25 C24 C12 121.8(4) . .
C23 C24 C12 119.8(4) . .
C24 C25 C26 121.9(4) . .
C27 C26 C25 117.8(4) . .
C27 C26 C19 120.8(3) . .
C25 C26 C19 121.4(3) . .
C22 C27 C26 121.9(4) . .
C28 O8 Co2 117.4(7) . .
C28 N1 C29 115.2(14) . .
C28 N1 C30 111.9(14) . .
C29 N1 C30 132.9(14) . .
O8 C28 N1 126.1(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O4 2.005(3) 1_455
Co1 O7 2.030(2) .
Co1 O6 2.051(5) 2_665
Co1 O1W 2.132(6) .
Co1 O2 2.140(3) .
Co1 O1 2.243(4) .
Co1 C1 2.507(4) .
Co2 O3 2.072(3) 7_465
Co2 O3 2.072(3) 1_455
Co2 O5 2.082(3) 2_665
Co2 O5 2.082(3) 8_756
Co2 O7 2.125(4) .
Co2 O8 2.127(5) .
O7 Co1 2.030(2) 7_565
O1 C1 1.251(6) .
O2 C1 1.231(6) .
O3 C8 1.221(5) .
O3 Co2 2.072(3) 1_655
O4 C8 1.253(5) .
O4 Co1 2.005(3) 1_655
O5 C15 1.241(5) .
O5 Co2 2.082(3) 2_664
O6 C15 1.248(6) .
O6 Co1 2.051(5) 2_664
C1 C2 1.513(6) .
C2 C7 1.365(7) .
C2 C3 1.370(7) .
C3 C4 1.389(6) .
C4 C5 1.355(7) .
C5 C6 1.361(6) .
C5 C22 1.504(5) .
C6 C7 1.397(6) .
C8 C9 1.516(6) .
C9 C10 1.355(7) .
C9 C14 1.389(6) .
C10 C11 1.387(6) .
C11 C12 1.380(6) .
C12 C13 1.390(7) .
C12 C24 1.497(6) .
C13 C14 1.373(5) .
C15 C16 1.486(7) .
C16 C21 1.385(7) .
C16 C17 1.423(6) .
C17 C18 1.357(7) .
C18 C19 1.378(7) .
C19 C20 1.406(6) .
C19 C26 1.483(6) .
C20 C21 1.373(6) .
C22 C27 1.381(6) .
C22 C23 1.382(6) .
C23 C24 1.423(5) .
C24 C25 1.376(6) .
C25 C26 1.402(5) .
C26 C27 1.399(5) .
O8 C28 1.248(10) .
N1 C28 1.397(9) .
N1 C29 1.589(17) .
N1 C30 1.604(18) .
