#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:35:16 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180188 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/84/7108469.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_7108469
loop_
_publ_author_name
'Fei-Yan Yi'
'Jian Zhang'
'Hai-Xia Zhang'
'Zhong-Ming Sun'
_publ_section_title
;
 Chiral transformations of achiral porous metal-organic frameworks via a
 stepwise approach
;
_journal_name_full               Chem.Commun.
_journal_page_first              10419
_journal_paper_doi               10.1039/c2cc35399g
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C76 H52 Co3 N8 O24'
_chemical_formula_weight         1638.05
_chemical_name_systematic
;
?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_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                 102.490(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.965(7)
_cell_length_b                   28.706(11)
_cell_length_c                   14.825(10)
_cell_measurement_temperature    273(2)
_cell_volume                     7049(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(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  0.0551
_diffrn_reflns_av_sigmaI/netI    0.1077
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19428
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_T_max  0.7448
_exptl_absorpt_correction_T_min  0.6182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.772
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brick
_exptl_crystal_F_000             1674
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.167
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_coef       0.0130(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         10917
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0789
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1332P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2062
_refine_ls_wR_factor_ref         0.2351
_reflns_number_gt                7099
_reflns_number_total             10917
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc35399g.txt
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      C2
_cod_database_code               7108469
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -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
Co1 Co 0.5000 0.30203(4) 0.0000 0.0414(3) Uani 1 2 d S
Co2 Co 0.39408(4) 0.40497(3) -0.00939(6) 0.0402(3) Uani 1 1 d .
O1 O 0.6531(4) 0.7555(2) 0.5269(4) 0.093(2) Uani 1 1 d .
O2 O 0.5000 0.6886(3) 0.5000 0.090(3) Uani 1 2 d S
O3 O 0.5403(4) 0.6435(2) 0.3038(4) 0.0874(18) Uani 1 1 d .
O4 O 0.6923(5) 0.7186(2) 0.3185(6) 0.112(3) Uani 1 1 d .
O5 O 0.8909(3) 0.79612(19) 0.9068(4) 0.0760(16) Uani 1 1 d .
O6 O 0.8334(3) 0.86527(17) 0.8795(4) 0.0601(14) Uani 1 1 d .
O7 O 0.8539(3) 0.86043(18) 0.0841(4) 0.0609(13) Uani 1 1 d .
O8 O 0.9397(3) 0.8009(2) 0.1069(4) 0.0775(16) Uani 1 1 d .
O11 O 0.5000 0.3722(2) 0.0000 0.059(2) Uani 1 2 d S
O9 O 0.4466(3) 0.4534(2) 0.0958(4) 0.0725(16) Uani 1 1 d .
O10 O 0.5779(3) 0.4537(2) 0.1028(4) 0.0724(17) Uani 1 1 d .
N3 N 0.5000 0.2280(3) 0.0000 0.062(2) Uani 1 2 d S
N1 N 0.4309(3) 0.0585(2) 0.0033(6) 0.073(2) Uani 1 1 d .
N2 N 0.5000 -0.0127(3) 0.0000 0.071(3) Uani 1 2 d S
N4 N 0.2173(3) -0.05930(18) 0.0151(4) 0.0505(15) Uani 1 1 d .
C1 C 0.5995(4) 0.7020(2) 0.4098(5) 0.0530(17) Uani 1 1 d .
C3 C 0.6168(5) 0.7332(3) 0.3338(6) 0.069(2) Uani 1 1 d .
H3A H 0.5751 0.7297 0.2780 0.083 Uiso 1 1 calc R
H3B H 0.6190 0.7655 0.3529 0.083 Uiso 1 1 calc R
C2 C 0.6597(6) 0.7091(3) 0.4980(6) 0.075(2) Uani 1 1 d .
H2A H 0.6492 0.6877 0.5447 0.090 Uiso 1 1 calc R
H2B H 0.7138 0.7034 0.4889 0.090 Uiso 1 1 calc R
C5 C 0.5164(5) 0.7144(3) 0.4254(5) 0.062(2) Uani 1 1 d .
H5A H 0.5142 0.7474 0.4384 0.075 Uiso 1 1 calc R
H5B H 0.4759 0.7077 0.3700 0.075 Uiso 1 1 calc R
C4 C 0.6037(5) 0.6513(3) 0.3843(5) 0.063(2) Uani 1 1 d .
H4A H 0.6559 0.6443 0.3708 0.075 Uiso 1 1 calc R
H4B H 0.5960 0.6316 0.4348 0.075 Uiso 1 1 calc R
C6 C 0.7000(6) 0.7693(3) 0.6115(6) 0.081(3) Uani 1 1 d .
C11 C 0.7597(7) 0.7433(3) 0.6626(7) 0.108(4) Uani 1 1 d .
H11A H 0.7718 0.7141 0.6419 0.129 Uiso 1 1 calc R
C20 C 0.5383(5) 0.5993(3) 0.2638(6) 0.073(2) Uani 1 1 d .
C21 C 0.6010(7) 0.5740(5) 0.2624(14) 0.184(9) Uani 1 1 d .
H21A H 0.6513 0.5830 0.2965 0.221 Uiso 1 1 calc R
C25 C 0.4669(6) 0.5822(4) 0.2250(10) 0.126(5) Uani 1 1 d .
H25A H 0.4209 0.5993 0.2277 0.151 Uiso 1 1 calc R
C13 C 0.7325(6) 0.7465(3) 0.2683(7) 0.086(3) Uani 1 1 d .
C14 C 0.7058(5) 0.7877(3) 0.2250(7) 0.081(3) Uani 1 1 d .
H14A H 0.6549 0.7989 0.2275 0.097 Uiso 1 1 calc R
C15 C 0.7522(5) 0.8119(3) 0.1794(6) 0.070(2) Uani 1 1 d .
H15A H 0.7348 0.8408 0.1543 0.084 Uiso 1 1 calc R
C16 C 0.8251(4) 0.7946(3) 0.1691(5) 0.0598(19) Uani 1 1 d .
C17 C 0.8507(6) 0.7539(3) 0.2081(8) 0.096(3) Uani 1 1 d .
H17A H 0.8995 0.7419 0.1997 0.115 Uiso 1 1 calc R
C18 C 0.8074(8) 0.7290(4) 0.2603(10) 0.136(6) Uani 1 1 d .
H18A H 0.8274 0.7013 0.2893 0.164 Uiso 1 1 calc R
C27 C 0.4314(4) 0.2031(2) 0.0011(7) 0.075(3) Uani 1 1 d .
H27A H 0.3838 0.2192 0.0014 0.090 Uiso 1 1 calc R
C28 C 0.4307(4) 0.1559(2) 0.0018(7) 0.080(3) Uani 1 1 d .
H28A H 0.3831 0.1402 0.0037 0.096 Uiso 1 1 d R
C29 C 0.5000 0.1309(3) 0.0000 0.063(3) Uani 1 2 d S
C30 C 0.5000 0.0803(4) 0.0000 0.068(3) Uani 1 2 d S
C31 C 0.4341(4) 0.0118(2) 0.0037(6) 0.066(2) Uani 1 1 d .
C12 C 0.8431(4) 0.8237(3) 0.8608(6) 0.0573(19) Uani 1 1 d .
C9 C 0.7911(4) 0.8042(3) 0.7737(5) 0.0613(18) Uani 1 1 d .
C8 C 0.7311(6) 0.8301(3) 0.7187(6) 0.092(3) Uani 1 1 d .
H8A H 0.7211 0.8601 0.7373 0.111 Uiso 1 1 calc R
C7 C 0.6863(6) 0.8134(3) 0.6381(7) 0.096(3) Uani 1 1 d .
H7A H 0.6468 0.8318 0.6016 0.115 Uiso 1 1 calc R
C10 C 0.8025(7) 0.7604(3) 0.7455(7) 0.095(3) Uani 1 1 d .
H10A H 0.8403 0.7414 0.7831 0.114 Uiso 1 1 calc R
C34 C 0.2196(4) -0.0123(3) 0.0117(7) 0.074(3) Uani 1 1 d .
H34A H 0.1726 0.0044 0.0113 0.089 Uiso 1 1 calc R
C33 C 0.2897(4) 0.0115(3) 0.0089(7) 0.073(2) Uani 1 1 d .
H33A H 0.2898 0.0439 0.0077 0.088 Uiso 1 1 calc R
C32 C 0.3594(4) -0.0127(2) 0.0078(6) 0.066(2) Uani 1 1 d .
C36 C 0.3571(4) -0.0609(2) 0.0127(7) 0.071(2) Uani 1 1 d .
H36A H 0.4034 -0.0784 0.0137 0.085 Uiso 1 1 calc R
C35 C 0.2867(4) -0.0821(2) 0.0163(6) 0.062(2) Uani 1 1 d .
H35A H 0.2863 -0.1145 0.0197 0.075 Uiso 1 1 calc R
C26 C 0.5154(4) 0.4700(3) 0.1192(5) 0.0541(18) Uani 1 1 d .
C19 C 0.8770(4) 0.8206(2) 0.1163(6) 0.0556(18) Uani 1 1 d .
C23 C 0.5223(4) 0.5155(3) 0.1707(5) 0.0561(18) Uani 1 1 d .
C24 C 0.4588(6) 0.5407(4) 0.1816(10) 0.122(5) Uani 1 1 d .
H24A H 0.4072 0.5292 0.1584 0.147 Uiso 1 1 calc R
C22 C 0.5934(6) 0.5325(5) 0.2091(12) 0.162(7) Uani 1 1 d .
H22A H 0.6397 0.5170 0.2013 0.195 Uiso 1 1 calc R
O2W O 0.657(3) 0.7476(18) 0.895(3) 0.51(2) Uiso 1 1 d .
C38 C 0.652(3) 0.6468(18) 1.042(3) 0.39(2) Uiso 1 1 d .
N5 N 0.702(3) 0.699(2) 0.961(3) 0.46(3) Uiso 1 1 d .
C37 C 0.700(4) 0.631(3) 0.928(4) 0.48(3) Uiso 1 1 d .
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
O11 Co1 O5 94.71(15) . 4_646
O11 Co1 O5 94.71(15) . 3_444
O5 Co1 O5 170.6(3) 4_646 3_444
O11 Co1 O8 90.88(17) . 3_445
O5 Co1 O8 90.4(3) 4_646 3_445
O5 Co1 O8 89.5(3) 3_444 3_445
O11 Co1 O8 90.88(17) . 4_645
O5 Co1 O8 89.5(3) 4_646 4_645
O5 Co1 O8 90.4(3) 3_444 4_645
O8 Co1 O8 178.2(3) 3_445 4_645
O11 Co1 N3 180.0 . .
O5 Co1 N3 85.29(15) 4_646 .
O5 Co1 N3 85.29(15) 3_444 .
O8 Co1 N3 89.12(17) 3_445 .
O8 Co1 N3 89.12(17) 4_645 .
O11 Co2 O6 94.60(17) . 3_444
O11 Co2 O10 91.80(18) . 2_655
O6 Co2 O10 89.2(2) 3_444 2_655
O11 Co2 O7 94.70(18) . 3_445
O6 Co2 O7 90.8(2) 3_444 3_445
O10 Co2 O7 173.5(2) 2_655 3_445
O11 Co2 N4 178.20(19) . 4
O6 Co2 N4 87.1(2) 3_444 4
O10 Co2 N4 88.8(2) 2_655 4
O7 Co2 N4 84.7(2) 3_445 4
O11 Co2 O9 91.65(18) . .
O6 Co2 O9 172.2(2) 3_444 .
O10 Co2 O9 86.0(3) 2_655 .
O7 Co2 O9 93.3(2) 3_445 .
N4 Co2 O9 86.7(2) 4 .
C6 O1 C2 118.3(7) . .
C5 O2 C5 116.6(9) 2_656 .
C20 O3 C4 116.0(7) . .
C13 O4 C3 119.3(7) . .
C12 O5 Co1 135.0(5) . 3_556
C12 O6 Co2 129.4(5) . 3_556
C19 O7 Co2 132.7(4) . 3
C19 O8 Co1 131.2(5) . 3
Co2 O11 Co2 124.0(3) 2_655 .
Co2 O11 Co1 117.99(15) 2_655 .
Co2 O11 Co1 117.99(15) . .
C26 O9 Co2 132.4(5) . .
C26 O10 Co2 135.5(5) . 2_655
C27 N3 C27 117.1(8) 2_655 .
C27 N3 Co1 121.4(4) 2_655 .
C27 N3 Co1 121.4(4) . .
C30 N1 C31 115.5(6) . .
C31 N2 C31 116.3(8) 2_655 .
C35 N4 C34 117.1(5) . .
C35 N4 Co2 122.1(4) . 4_545
C34 N4 Co2 120.6(4) . 4_545
C2 C1 C4 107.0(7) . .
C2 C1 C3 111.5(7) . .
C4 C1 C3 110.8(6) . .
C2 C1 C5 108.4(6) . .
C4 C1 C5 111.0(6) . .
C3 C1 C5 108.1(7) . .
O4 C3 C1 105.8(7) . .
O1 C2 C1 108.2(7) . .
O2 C5 C1 110.1(6) . .
O3 C4 C1 106.9(7) . .
C11 C6 C7 120.4(8) . .
C11 C6 O1 124.3(8) . .
C7 C6 O1 115.2(8) . .
C6 C11 C10 119.4(8) . .
C21 C20 C25 117.8(9) . .
C21 C20 O3 124.9(9) . .
C25 C20 O3 117.3(8) . .
C20 C21 C22 120.3(10) . .
C20 C25 C24 121.8(9) . .
O4 C13 C14 127.1(8) . .
O4 C13 C18 113.8(9) . .
C14 C13 C18 119.0(8) . .
C15 C14 C13 120.9(8) . .
C14 C15 C16 120.7(8) . .
C17 C16 C15 119.0(7) . .
C17 C16 C19 119.4(7) . .
C15 C16 C19 121.6(7) . .
C16 C17 C18 122.4(9) . .
C17 C18 C13 117.8(10) . .
C28 C27 N3 122.1(7) . .
C27 C28 C29 120.6(7) . .
C28 C29 C28 117.5(9) 2_655 .
C28 C29 C30 121.3(4) 2_655 .
C28 C29 C30 121.3(4) . .
N1 C30 N1 124.4(9) 2_655 .
N1 C30 C29 117.8(5) 2_655 .
N1 C30 C29 117.8(5) . .
N2 C31 N1 124.1(6) . .
N2 C31 C32 119.4(6) . .
N1 C31 C32 116.5(6) . .
O5 C12 O6 126.8(7) . .
O5 C12 C9 115.4(7) . .
O6 C12 C9 117.8(7) . .
C10 C9 C8 117.2(7) . .
C10 C9 C12 121.0(8) . .
C8 C9 C12 121.8(7) . .
C7 C8 C9 122.1(8) . .
C8 C7 C6 119.1(8) . .
C9 C10 C11 121.7(9) . .
N4 C34 C33 121.8(6) . .
C32 C33 C34 119.9(7) . .
C33 C32 C36 118.0(6) . .
C33 C32 C31 120.9(6) . .
C36 C32 C31 121.1(6) . .
C35 C36 C32 119.2(6) . .
N4 C35 C36 123.9(6) . .
O10 C26 O9 126.8(7) . .
O10 C26 C23 117.0(6) . .
O9 C26 C23 116.2(6) . .
O8 C19 O7 124.9(6) . .
O8 C19 C16 116.6(6) . .
O7 C19 C16 118.5(6) . .
C22 C23 C24 115.9(8) . .
C22 C23 C26 120.4(8) . .
C24 C23 C26 123.7(7) . .
C23 C24 C25 122.3(9) . .
C23 C22 C21 121.1(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O11 2.013(6) .
Co1 O5 2.064(5) 4_646
Co1 O5 2.064(5) 3_444
Co1 O8 2.065(5) 3_445
Co1 O8 2.065(5) 4_645
Co1 N3 2.125(8) .
Co2 O11 2.007(3) .
Co2 O6 2.083(5) 3_444
Co2 O10 2.094(5) 2_655
Co2 O7 2.104(5) 3_445
Co2 N4 2.136(5) 4
Co2 O9 2.136(5) .
O1 C6 1.389(10) .
O1 C2 1.411(10) .
O2 C5 1.408(9) 2_656
O2 C5 1.408(9) .
O3 C20 1.399(9) .
O3 C4 1.441(10) .
O4 C13 1.372(10) .
O4 C3 1.411(10) .
O5 C12 1.229(8) .
O5 Co1 2.064(5) 3_556
O6 C12 1.243(8) .
O6 Co2 2.083(5) 3_556
O7 C19 1.268(8) .
O7 Co2 2.104(5) 3
O8 C19 1.238(8) .
O8 Co1 2.065(5) 3
O11 Co2 2.007(3) 2_655
O9 C26 1.237(8) .
O10 C26 1.231(8) .
O10 Co2 2.094(5) 2_655
N3 C27 1.367(8) 2_655
N3 C27 1.367(8) .
N1 C30 1.338(7) .
N1 C31 1.343(9) .
N2 C31 1.332(8) 2_655
N2 C31 1.332(8) .
N4 C35 1.344(8) .
N4 C34 1.350(9) .
N4 Co2 2.136(5) 4_545
C1 C2 1.489(11) .
C1 C4 1.508(10) .
C1 C3 1.515(10) .
C1 C5 1.520(10) .
C6 C11 1.351(13) .
C6 C7 1.362(12) .
C11 C10 1.376(13) .
C20 C21 1.291(14) .
C20 C25 1.317(13) .
C21 C22 1.420(14) .
C25 C24 1.345(13) .
C13 C14 1.375(12) .
C13 C18 1.396(14) .
C14 C15 1.338(11) .
C15 C16 1.373(10) .
C16 C17 1.335(11) .
C16 C19 1.497(9) .
C17 C18 1.377(12) .
C27 C28 1.357(10) .
C28 C29 1.383(8) .
C29 C28 1.383(8) 2_655
C29 C30 1.453(14) .
C30 N1 1.338(7) 2_655
C31 C32 1.461(9) .
C12 C9 1.507(10) .
C9 C10 1.351(12) .
C9 C8 1.376(11) .
C8 C7 1.357(11) .
C34 C33 1.382(9) .
C33 C32 1.375(9) .
C32 C36 1.386(10) .
C36 C35 1.353(9) .
C26 C23 1.506(10) .
C23 C22 1.311(12) .
C23 C24 1.336(12) .
O2W N5 1.78(6) .
