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#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/47/1514754.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_1514754
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            'C79.5 H115.5 Co3 N8.5 O34.5'
_chemical_formula_weight         1919.09
_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                   17.564(4)
_cell_length_b                   25.629(5)
_cell_length_c                   20.800(4)
_cell_measurement_temperature    173(2)
_cell_volume                     9363(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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.1325
_diffrn_reflns_av_sigmaI/netI    0.1215
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            84131
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.611
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4036
_refine_diff_density_max         1.109
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         10847
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.2561
_refine_ls_R_factor_gt           0.1113
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1853P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2894
_refine_ls_wR_factor_ref         0.3548
_reflns_number_gt                4031
_reflns_number_total             10847
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc51379c.txt
_cod_data_source_block           1a
_cod_original_sg_symbol_H-M      Pnma
_cod_original_formula_sum        'C79.50 H115.50 Co3 N8.50 O34.50'
_cod_database_code               1514754
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 0.99689(4) 0.68198(4) -0.43835(6) 0.1005(5) Uani 1 1 d .
Co2 Co 0.88638(5) 0.7500 -0.33774(5) 0.0682(4) Uani 1 2 d S
O1W O 0.9915(5) 0.7500 -0.5231(5) 0.339(14) Uani 1 2 d S
O7 O 0.9812(3) 0.7500 -0.3989(3) 0.0906(19) Uani 1 2 d S
O1 O 1.0670(3) 0.6216(5) -0.4829(4) 0.235(5) Uani 1 1 d .
O2 O 1.1198(4) 0.6864(3) -0.4412(5) 0.159(3) Uani 1 1 d .
O3 O 1.8270(2) 0.69552(19) -0.3853(2) 0.0969(17) Uani 1 1 d .
O4 O 1.8950(2) 0.6594(3) -0.4644(3) 0.138(2) Uani 1 1 d .
O5 O 1.5643(2) 0.30783(18) -0.7828(2) 0.0904(13) Uani 1 1 d .
O6 O 1.4955(3) 0.3559(2) -0.8529(3) 0.129(2) Uani 1 1 d .
C1 C 1.1203(5) 0.6486(6) -0.4732(5) 0.150(5) Uani 1 1 d .
C2 C 1.2008(4) 0.6277(5) -0.4903(5) 0.149(4) Uani 1 1 d .
C3 C 1.2606(4) 0.6560(4) -0.4861(5) 0.134(3) Uani 1 1 d .
H3A H 1.2548 0.6893 -0.4691 0.161 Uiso 1 1 calc R
C4 C 1.3332(4) 0.6412(4) -0.5048(5) 0.168(5) Uani 1 1 d .
H4A H 1.3740 0.6642 -0.5020 0.202 Uiso 1 1 calc R
C5 C 1.3424(4) 0.5921(4) -0.5273(5) 0.138(4) Uani 1 1 d .
C6 C 1.2824(4) 0.5578(5) -0.5271(6) 0.193(6) Uani 1 1 d .
H6A H 1.2879 0.5232 -0.5397 0.231 Uiso 1 1 calc R
C7 C 1.2111(4) 0.5785(6) -0.5063(5) 0.181(6) Uani 1 1 d .
H7A H 1.1696 0.5560 -0.5041 0.217 Uiso 1 1 calc R
C8 C 1.8313(3) 0.6697(3) -0.4277(5) 0.098(3) Uani 1 1 d .
C9 C 1.7620(3) 0.6412(3) -0.4631(4) 0.099(2) Uani 1 1 d .
C10 C 1.7642(3) 0.6147(4) -0.5162(4) 0.120(3) Uani 1 1 d .
H10A H 1.8108 0.6099 -0.5367 0.144 Uiso 1 1 calc R
C11 C 1.6975(4) 0.5926(4) -0.5441(5) 0.139(4) Uani 1 1 d .
H11A H 1.6988 0.5779 -0.5850 0.166 Uiso 1 1 calc R
C12 C 1.6297(3) 0.5938(3) -0.5084(4) 0.100(2) Uani 1 1 d .
C13 C 1.6294(3) 0.6196(3) -0.4509(4) 0.100(2) Uani 1 1 d .
H13A H 1.5843 0.6220 -0.4277 0.121 Uiso 1 1 calc R
C14 C 1.6951(3) 0.6423(3) -0.4263(4) 0.096(2) Uani 1 1 d .
H14A H 1.6947 0.6581 -0.3860 0.115 Uiso 1 1 calc R
C15 C 1.5243(3) 0.3467(3) -0.7970(5) 0.102(3) Uani 1 1 d .
C16 C 1.5155(3) 0.3860(3) -0.7465(4) 0.094(2) Uani 1 1 d .
C17 C 1.4606(4) 0.4269(3) -0.7547(4) 0.112(3) Uani 1 1 d .
H17A H 1.4286 0.4269 -0.7904 0.135 Uiso 1 1 calc R
C18 C 1.4554(3) 0.4651(3) -0.7111(4) 0.120(3) Uani 1 1 d .
H18A H 1.4201 0.4915 -0.7180 0.144 Uiso 1 1 calc R
C19 C 1.5014(3) 0.4676(3) -0.6540(4) 0.108(3) Uani 1 1 d .
C20 C 1.5567(3) 0.4252(3) -0.6478(4) 0.099(2) Uani 1 1 d .
H20A H 1.5891 0.4239 -0.6125 0.119 Uiso 1 1 calc R
C21 C 1.5605(3) 0.3876(3) -0.6941(4) 0.092(2) Uani 1 1 d .
H21A H 1.5967 0.3614 -0.6892 0.110 Uiso 1 1 calc R
C22 C 1.4209(3) 0.5702(3) -0.5467(4) 0.104(3) Uani 1 1 d .
C23 C 1.4865(3) 0.5904(3) -0.5204(4) 0.111(3) Uani 1 1 d .
H23A H 1.4825 0.6173 -0.4906 0.133 Uiso 1 1 calc R
C24 C 1.5595(3) 0.5718(3) -0.5368(4) 0.099(2) Uani 1 1 d .
C25 C 1.5630(3) 0.5316(3) -0.5782(4) 0.104(2) Uani 1 1 d .
H25A H 1.6103 0.5172 -0.5874 0.124 Uiso 1 1 calc R
C26 C 1.4964(3) 0.5096(3) -0.6090(4) 0.105(3) Uani 1 1 d .
C27 C 1.4270(3) 0.5307(3) -0.5883(4) 0.114(3) Uani 1 1 d .
H27A H 1.3824 0.5162 -0.6045 0.136 Uiso 1 1 calc R
O8 O 0.7965(3) 0.7500 -0.2703(3) 0.0941(19) Uani 1 2 d SD
N1 N 0.7144(13) 0.6958(7) -0.2098(11) 0.215(10) Uani 0.50 1 d PD
C28 C 0.7732(9) 0.7036(7) -0.2519(12) 0.209(13) Uani 0.50 1 d PD
H28A H 0.7980 0.6744 -0.2684 0.251 Uiso 0.50 1 calc PR
C29 C 0.6880(12) 0.7500 -0.1860(17) 0.277(15) Uani 1 2 d SD
C30 C 0.7187(11) 0.6334(11) -0.2001(17) 0.49(4) Uani 0.50 1 d PD
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
O7 Co1 O4 104.6(2) . 1_455
O7 Co1 O6 94.0(3) . 2_765
O4 Co1 O6 99.3(3) 1_455 2_765
O7 Co1 O2 96.1(3) . .
O4 Co1 O2 157.0(3) 1_455 .
O6 Co1 O2 89.0(3) 2_765 .
O7 Co1 O1 153.3(3) . .
O4 Co1 O1 100.9(3) 1_455 .
O6 Co1 O1 89.7(3) 2_765 .
O2 Co1 O1 57.5(3) . .
O7 Co1 C1 124.4(4) . .
O4 Co1 C1 128.8(3) 1_455 .
O6 Co1 C1 91.9(3) 2_765 .
O2 Co1 C1 28.8(3) . .
O1 Co1 C1 28.9(3) . .
O3 Co2 O3 88.3(3) 1_455 7_475
O3 Co2 O5 89.5(2) 1_455 2_765
O3 Co2 O5 173.19(17) 7_475 2_765
O3 Co2 O5 173.19(17) 1_455 8_866
O3 Co2 O5 89.5(2) 7_475 8_866
O5 Co2 O5 91.9(3) 2_765 8_866
O3 Co2 O7 96.54(18) 1_455 .
O3 Co2 O7 96.54(18) 7_475 .
O5 Co2 O7 90.12(18) 2_765 .
O5 Co2 O7 90.12(18) 8_866 .
O3 Co2 O8 86.50(18) 1_455 .
O3 Co2 O8 86.50(18) 7_475 .
O5 Co2 O8 86.92(18) 2_765 .
O5 Co2 O8 86.92(18) 8_866 .
O7 Co2 O8 175.7(3) . .
Co1 O7 Co1 127.2(3) . 7_575
Co1 O7 Co2 111.61(14) . .
Co1 O7 Co2 111.61(14) 7_575 .
C1 O1 Co1 87.7(8) . .
C1 O2 Co1 88.9(7) . .
C8 O3 Co2 140.9(4) . 1_655
C8 O4 Co1 122.0(5) . 1_655
C15 O5 Co2 132.6(5) . 2_764
C15 O6 Co1 132.5(5) . 2_764
O2 C1 O1 125.0(10) . .
O2 C1 C2 114.9(9) . .
O1 C1 C2 118.7(12) . .
O2 C1 Co1 62.4(6) . .
O1 C1 Co1 63.4(6) . .
C2 C1 Co1 175.9(7) . .
C3 C2 C7 116.6(8) . .
C3 C2 C1 122.3(10) . .
C7 C2 C1 120.9(10) . .
C2 C3 C4 125.5(9) . .
C5 C4 C3 117.5(8) . .
C4 C5 C6 120.2(8) . .
C4 C5 C22 122.5(7) . .
C6 C5 C22 117.0(9) . .
C5 C6 C7 115.9(10) . .
C2 C7 C6 123.6(9) . .
O3 C8 O4 127.8(5) . .
O3 C8 C9 126.0(7) . .
O4 C8 C9 105.9(7) . .
C10 C9 C14 120.1(6) . .
C10 C9 C8 127.4(6) . .
C14 C9 C8 112.1(7) . .
C9 C10 C11 121.9(6) . .
C12 C11 C10 118.3(7) . .
C13 C12 C11 118.5(5) . .
C13 C12 C24 122.0(5) . .
C11 C12 C24 119.2(6) . .
C12 C13 C14 121.4(6) . .
C13 C14 C9 119.1(6) . .
O5 C15 O6 125.2(7) . .
O5 C15 C16 115.9(8) . .
O6 C15 C16 118.8(7) . .
C21 C16 C17 117.9(7) . .
C21 C16 C15 122.8(7) . .
C17 C16 C15 119.1(7) . .
C18 C17 C16 119.9(7) . .
C17 C18 C19 123.7(7) . .
C26 C19 C18 122.6(7) . .
C26 C19 C20 122.9(7) . .
C18 C19 C20 114.4(7) . .
C21 C20 C19 119.7(7) . .
C16 C21 C20 124.4(6) . .
C27 C22 C23 118.4(6) . .
C27 C22 C5 121.2(6) . .
C23 C22 C5 120.5(6) . .
C22 C23 C24 122.6(6) . .
C25 C24 C23 117.1(5) . .
C25 C24 C12 120.7(5) . .
C23 C24 C12 122.2(6) . .
C24 C25 C26 123.1(6) . .
C27 C26 C19 123.0(5) . .
C27 C26 C25 114.6(6) . .
C19 C26 C25 122.3(5) . .
C22 C27 C26 124.2(6) . .
C28 O8 C28 129.6(18) . 7_575
C28 O8 Co2 115.2(9) . .
C28 O8 Co2 115.2(9) 7_575 .
C28 N1 C29 107.5(18) . .
C28 N1 C30 100.9(16) . .
C29 N1 C30 150(2) . .
O8 C28 N1 123.5(17) . .
N1 C29 N1 128(2) . 7_575
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O7 1.946(3) .
Co1 O4 1.958(4) 1_455
Co1 O6 2.030(6) 2_765
Co1 O2 2.162(7) .
Co1 O1 2.184(8) .
Co1 C1 2.440(10) .
Co2 O3 2.005(4) 1_455
Co2 O3 2.005(4) 7_475
Co2 O5 2.062(4) 2_765
Co2 O5 2.062(4) 8_866
Co2 O7 2.096(5) .
Co2 O8 2.112(6) .
O7 Co1 1.946(3) 7_575
O1 C1 1.181(12) .
O2 C1 1.175(11) .
O3 C8 1.104(8) .
O3 Co2 2.005(4) 1_655
O4 C8 1.380(9) .
O4 Co1 1.958(4) 1_655
O5 C15 1.255(8) .
O5 Co2 2.062(4) 2_764
O6 C15 1.290(10) .
O6 Co1 2.030(6) 2_764
C1 C2 1.554(12) .
C2 C3 1.280(11) .
C2 C7 1.316(15) .
C3 C4 1.386(10) .
C4 C5 1.352(12) .
C5 C6 1.372(12) .
C5 C22 1.542(9) .
C6 C7 1.428(12) .
C8 C9 1.600(9) .
C9 C10 1.297(9) .
C9 C14 1.402(8) .
C10 C11 1.425(9) .
C11 C12 1.403(9) .
C12 C13 1.368(9) .
C12 C24 1.478(8) .
C13 C14 1.390(8) .
C15 C16 1.462(10) .
C16 C21 1.346(9) .
C16 C17 1.437(9) .
C17 C18 1.338(10) .
C18 C19 1.437(10) .
C19 C26 1.429(10) .
C19 C20 1.463(10) .
C20 C21 1.363(9) .
C22 C27 1.336(9) .
C22 C23 1.377(8) .
C23 C24 1.409(8) .
C24 C25 1.344(9) .
C25 C26 1.447(8) .
C26 C27 1.401(8) .
O8 C28 1.315(15) .
O8 C28 1.315(15) 7_575
N1 C28 1.368(16) .
N1 C29 1.546(16) .
N1 C30 1.615(19) .
C29 N1 1.546(16) 7_575
