#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:49:35 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179349 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/46/4324620.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_4324620
loop_
_publ_author_name
'Qing Chen'
'Jian-Bin Lin'
'Wei Xue'
'Ming-Hua Zeng'
'Xiao-Ming Chen'
_publ_section_title
;
 A Porous Coordination Polymer Assembled from 8-Connected {CoII3(OH)}
 Clusters and Isonicotinate: Multiple Active Metal Sites, Apical Ligand
 Substitution, H2 Adsorption, and Magnetism
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2321
_journal_page_last               2328
_journal_paper_doi               10.1021/ic102015g
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C30 H35 Co3 N5 O15'
_chemical_formula_weight         882.42
_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                   18.986(4)
_cell_length_b                   19.683(4)
_cell_length_c                   12.081(2)
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     4514.7(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21372
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    1.150
_exptl_absorpt_correction_T_max  0.8026
_exptl_absorpt_correction_T_min  0.6889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       block
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.810
_refine_diff_density_min         -2.792
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4539
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0882
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1429P)²+27.4063P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2559
_refine_ls_wR_factor_ref         0.2653
_reflns_number_gt                3713
_reflns_number_total             4539
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102015g_si_001_2.cif
_cod_data_source_block           1
_cod_original_cell_volume        4514.6(15)
_cod_database_code               4324620
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.19077(5) 0.66208(4) 0.17025(7) 0.0282(3) Uani 1 1 d . . .
Co2 Co 0.15669(6) 0.7500 0.42999(9) 0.0260(3) Uani 1 2 d S . .
C1 C 0.2135(5) 0.4618(4) 0.6118(7) 0.0519(19) Uani 1 1 d . . .
H1A H 0.1870 0.4442 0.6720 0.062 Uiso 1 1 calc R . .
C2 C 0.1891(5) 0.5182(4) 0.5583(6) 0.0505(19) Uani 1 1 d . . .
H2A H 0.1470 0.5398 0.5822 0.061 Uiso 1 1 calc R . .
C3 C 0.2268(4) 0.5440(3) 0.4675(5) 0.0358(14) Uani 1 1 d . . .
C4 C 0.2884(5) 0.5111(5) 0.4381(7) 0.061(2) Uani 1 1 d . . .
H4A H 0.3162 0.5271 0.3781 0.073 Uiso 1 1 calc R . .
C5 C 0.3087(5) 0.4548(5) 0.4976(8) 0.063(3) Uani 1 1 d . . .
H5A H 0.3507 0.4325 0.4754 0.076 Uiso 1 1 calc R . .
C6 C 0.2018(4) 0.6044(3) 0.4032(5) 0.0334(14) Uani 1 1 d . . .
C7 C 0.5079(4) 0.6921(4) 0.0790(8) 0.053(2) Uani 1 1 d . . .
H7B H 0.5325 0.6504 0.0710 0.063 Uiso 1 1 calc R . .
C8 C 0.4353(4) 0.6902(4) 0.0994(8) 0.056(2) Uani 1 1 d . . .
H8A H 0.4113 0.6480 0.1060 0.068 Uiso 1 1 calc R . .
C9 C 0.3996(5) 0.7500 0.1095(7) 0.0321(19) Uani 1 2 d S . .
C10 C 0.3220(6) 0.7500 0.1409(15) 0.070(2) Uani 1 2 d SU . .
C11 C 0.1912(10) 0.7017(9) -0.3271(12) 0.054(4) Uani 0.50 1 d P . 1
H11A H 0.2172 0.6679 -0.3656 0.064 Uiso 0.50 1 calc PR . 1
C11' C 0.1253(10) 0.7012(8) -0.3297(10) 0.047(4) Uani 0.50 1 d P . 2
H11B H 0.1018 0.6666 -0.3701 0.057 Uiso 0.50 1 calc PR . 2
C12 C 0.1890(11) 0.6989(9) -0.2143(12) 0.058(5) Uani 0.50 1 d P . 1
H12A H 0.2096 0.6616 -0.1764 0.070 Uiso 0.50 1 calc PR . 1
C12' C 0.1237(9) 0.6984(7) -0.2149(11) 0.044(3) Uani 0.50 1 d P . 2
H12B H 0.1005 0.6622 -0.1777 0.053 Uiso 0.50 1 calc PR . 2
C13 C 0.1569(5) 0.7500 -0.1556(7) 0.034(2) Uani 1 2 d S . .
C14 C 0.1593(5) 0.7500 -0.0287(7) 0.036(2) Uani 1 2 d S . .
N1 N 0.2748(3) 0.4295(3) 0.5824(5) 0.0414(13) Uani 1 1 d . . .
N2 N 0.5441(4) 0.7500 0.0704(6) 0.0308(15) Uani 1 2 d S . .
N3 N 0.1584(5) 0.7500 -0.3865(6) 0.0369(18) Uani 1 2 d S . .
O1 O 0.1563(3) 0.7500 0.2550(5) 0.0235(11) Uani 1 2 d S . .
O2 O 0.1599(3) 0.6451(2) 0.4504(4) 0.0377(11) Uani 1 1 d . . .
O3 O 0.2248(3) 0.6099(3) 0.3070(4) 0.0474(13) Uani 1 1 d . . .
O4 O 0.2928(3) 0.6948(3) 0.1522(7) 0.076(2) Uani 1 1 d U . .
O5 O 0.1591(5) 0.6946(3) 0.0156(4) 0.076(2) Uani 1 1 d . . .
O7 O 0.2705(5) 0.7500 0.4179(8) 0.092(3) Uani 1 2 d SDU . .
H7A H 0.2767 0.7610 0.3506 0.110 Uiso 0.50 1 d PR . .
C17 C 0.3288(5) 0.7796 0.4701(8) 0.101(3) Uani 0.50 1 d PRDU . .
H17A H 0.3282 0.7695 0.5478 0.122 Uiso 0.50 1 d PR . .
H17B H 0.3278 0.8280 0.4609 0.122 Uiso 0.50 1 d PR . .
C18 C 0.3943(7) 0.7500 0.4151(15) 0.109(4) Uani 1 2 d SDU . .
H18A H 0.4354 0.7693 0.4493 0.164 Uiso 0.50 1 d PR . .
H18B H 0.3948 0.7016 0.4250 0.164 Uiso 0.50 1 d PR . .
H18C H 0.3944 0.7605 0.3375 0.164 Uiso 0.50 1 d PR . .
O6 O 0.0872(3) 0.6161(4) 0.1878(7) 0.0802(18) Uani 1 1 d DU . .
H6A H 0.0783 0.6140 0.2567 0.096 Uiso 1 1 d R . .
C15 C 0.0249(5) 0.6390(6) 0.1397(12) 0.096(2) Uani 1 1 d DU . 1
H15A H 0.0356 0.6710 0.0788 0.116 Uiso 1 1 calc R . 1
H15B H -0.0041 0.6629 0.1955 0.116 Uiso 1 1 calc R . 1
C16 C -0.0148(8) 0.5779(8) 0.0951(14) 0.130(3) Uani 1 1 d DU . 1
H16A H -0.0589 0.5931 0.0608 0.194 Uiso 1 1 calc R . 1
H16B H -0.0254 0.5466 0.1559 0.194 Uiso 1 1 calc R . 1
H16C H 0.0142 0.5547 0.0397 0.194 Uiso 1 1 calc R . 1
N4 N 0.0127(12) 0.5005(12) 0.381(2) 0.220(10) Uani 0.50 1 d PDU A 1
O8 O 0.0669(12) 0.5093(10) 0.3285(18) 0.141(8) Uani 0.50 1 d PDU A 1
O9 O -0.0313(16) 0.460(2) 0.347(3) 0.270(13) Uani 0.50 1 d PDU A 1
O10 O 0.0014(18) 0.5313(14) 0.467(2) 0.227(10) Uani 0.50 1 d PDU . 1
H1B H 0.115(5) 0.7500 0.240(7) 0.02(2) Uiso 1 2 d S B 1
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
O3 Co1 O4 86.8(3) . .
O3 Co1 O5 167.6(2) . .
O4 Co1 O5 94.7(3) . .
O3 Co1 O1 96.73(19) . .
O4 Co1 O1 95.0(2) . .
O5 Co1 O1 95.4(2) . .
O3 Co1 O6 89.9(3) . .
O4 Co1 O6 173.7(3) . .
O5 Co1 O6 87.4(3) . .
O1 Co1 O6 90.8(3) . .
O3 Co1 N1 83.4(2) . 2_564
O4 Co1 N1 85.7(3) . 2_564
O5 Co1 N1 84.5(2) . 2_564
O1 Co1 N1 179.4(2) . 2_564
O6 Co1 N1 88.6(3) . 2_564
O2 Co2 O2 166.0(3) . 7_575
O2 Co2 O1 96.82(13) . .
O2 Co2 O1 96.82(13) 7_575 .
O2 Co2 N2 91.70(14) . 6_556
O2 Co2 N2 91.70(14) 7_575 6_556
O1 Co2 N2 89.7(3) . 6_556
O2 Co2 O7 88.78(14) . .
O2 Co2 O7 88.78(14) 7_575 .
O1 Co2 O7 86.3(3) . .
N2 Co2 O7 176.0(3) 6_556 .
O2 Co2 N3 83.16(13) . 1_556
O2 Co2 N3 83.16(13) 7_575 1_556
O1 Co2 N3 179.4(3) . 1_556
N2 Co2 N3 91.0(3) 6_556 1_556
O7 Co2 N3 93.0(4) . 1_556
C2 C1 N1 122.8(8) . .
C2 C1 H1A 118.6 . .
N1 C1 H1A 118.6 . .
C1 C2 C3 119.3(7) . .
C1 C2 H2A 120.3 . .
C3 C2 H2A 120.3 . .
C4 C3 C2 117.5(6) . .
C4 C3 C6 120.5(6) . .
C2 C3 C6 122.0(6) . .
C5 C4 C3 118.7(8) . .
C5 C4 H4A 120.7 . .
C3 C4 H4A 120.7 . .
N1 C5 C4 125.3(8) . .
N1 C5 H5A 117.3 . .
C4 C5 H5A 117.3 . .
O3 C6 O2 125.8(6) . .
O3 C6 C3 116.2(6) . .
O2 C6 C3 117.9(6) . .
N2 C7 C8 122.9(7) . .
N2 C7 H7B 118.6 . .
C8 C7 H7B 118.6 . .
C9 C8 C7 118.8(7) . .
C9 C8 H8A 120.6 . .
C7 C8 H8A 120.6 . .
C8 C9 C8 119.4(9) . 7_575
C8 C9 C10 120.2(5) . .
C8 C9 C10 120.2(5) 7_575 .
O4 C10 O4 124.6(11) . 7_575
O4 C10 C9 117.7(5) . .
O4 C10 C9 117.7(5) 7_575 .
N3 C11 C12 123.1(14) . .
N3 C11 C11 45.0(8) . 7_575
C12 C11 C11 92.3(11) . 7_575
N3 C11 H11A 118.4 . .
C12 C11 H11A 118.4 . .
C11 C11 H11A 134.5 7_575 .
N3 C11' C12' 123.5(13) . .
N3 C11' C11' 44.0(8) . 7_575
C12' C11' C11' 92.3(9) . 7_575
N3 C11' H11B 118.3 . .
C12' C11' H11B 118.3 . .
C11' C11' H11B 135.8 7_575 .
C11 C12 C13 120.0(14) . .
C11 C12 C12 87.7(11) . 7_575
C13 C12 C12 42.9(9) . 7_575
C11 C12 H12A 120.0 . .
C13 C12 H12A 120.0 . .
C12 C12 H12A 140.6 7_575 .
C11' C12' C13 118.3(13) . .
C11' C12' C12' 87.7(9) . 7_575
C13 C12' C12' 43.2(7) . 7_575
C11' C12' H12B 120.9 . .
C13 C12' H12B 120.9 . .
C12' C12' H12B 138.5 7_575 .
C12 C13 C12 94.2(17) . 7_575
C12 C13 C12' 53.2(11) . .
C12 C13 C12' 118.0(10) 7_575 .
C12 C13 C12' 118.0(10) . 7_575
C12 C13 C12' 53.2(11) 7_575 7_575
C12' C13 C12' 93.6(14) . 7_575
C12 C13 C14 120.2(8) . .
C12 C13 C14 120.2(8) 7_575 .
C12' C13 C14 121.8(8) . .
C12' C13 C14 121.8(8) 7_575 .
O5 C14 O5 127.7(9) . 7_575
O5 C14 C13 116.1(5) . .
O5 C14 C13 116.1(5) 7_575 .
C5 N1 C1 116.3(6) . .
C5 N1 Co1 123.1(5) . 2_565
C1 N1 Co1 120.6(5) . 2_565
C7 N2 C7 117.3(8) . 7_575
C7 N2 Co2 121.0(4) . 6_656
C7 N2 Co2 121.0(4) 7_575 6_656
C11' N3 C11' 91.9(15) . 7_575
C11' N3 C11 116.9(10) . 7_575
C11' N3 C11 55.6(11) 7_575 7_575
C11' N3 C11 55.6(11) . .
C11' N3 C11 116.9(10) 7_575 .
C11 N3 C11 90.1(16) 7_575 .
C11' N3 Co2 120.4(7) . 1_554
C11' N3 Co2 120.4(7) 7_575 1_554
C11 N3 Co2 122.7(7) 7_575 1_554
C11 N3 Co2 122.7(7) . 1_554
Co1 O1 Co1 109.9(3) . 7_575
Co1 O1 Co2 118.90(16) . .
Co1 O1 Co2 118.90(16) 7_575 .
Co1 O1 H1B 101(4) . .
Co1 O1 H1B 101(4) 7_575 .
Co2 O1 H1B 104(6) . .
C6 O2 Co2 126.4(4) . .
C6 O3 Co1 133.2(5) . .
C10 O4 Co1 135.7(6) . .
C14 O5 Co1 132.6(6) . .
C17 O7 C17 49.1 7_575 .
C17 O7 Co2 139.3(2) 7_575 .
C17 O7 Co2 139.3(2) . .
C17 O7 H7A 115.2 7_575 .
C17 O7 H7A 102.4 . .
Co2 O7 H7A 101.7 . .
C17 C17 O7 65.5 7_575 .
C17 C17 C18 67.58(14) 7_575 .
O7 C17 C18 106.9(6) . .
C17 C17 H17A 78.1 7_575 .
O7 C17 H17A 110.2 . .
C18 C17 H17A 110.9 . .
C17 C17 H17B 173.3 7_575 .
O7 C17 H17B 110.2 . .
C18 C17 H17B 110.1 . .
H17A C17 H17B 108.5 . .
C17 C18 C17 44.8(3) . 7_575
C17 C18 H18A 108.9 . .
C17 C18 H18A 128.8 7_575 .
C17 C18 H18B 109.4 . .
C17 C18 H18B 64.9 7_575 .
H18A C18 H18B 109.5 . .
C17 C18 H18C 110.1 . .
C17 C18 H18C 120.5 7_575 .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C15 O6 Co1 126.3(7) . .
C15 O6 H6A 104.9 . .
Co1 O6 H6A 107.1 . .
O6 C15 C16 108.3(10) . .
O6 C15 H15A 110.0 . .
C16 C15 H15A 110.0 . .
O6 C15 H15B 110.0 . .
C16 C15 H15B 110.1 . .
H15A C15 H15B 108.4 . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.4 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
O8 N4 O10 121.1(13) . .
O8 N4 O9 119.9(12) . .
O10 N4 O9 119.0(12) . .
N4 O10 O10 93(3) . 5_566
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O3 2.050(5) .
Co1 O4 2.053(6) .
Co1 O5 2.064(5) .
Co1 O1 2.114(3) .
Co1 O6 2.176(7) .
Co1 N1 2.192(5) 2_564
Co2 O2 2.080(4) .
Co2 O2 2.080(4) 7_575
Co2 O1 2.114(6) .
Co2 N2 2.138(7) 6_556
Co2 O7 2.165(9) .
Co2 N3 2.218(8) 1_556
C1 C2 1.366(11) .
C1 N1 1.372(10) .
C1 H1A 0.9500 .
C2 C3 1.405(10) .
C2 H2A 0.9500 .
C3 C4 1.384(11) .
C3 C6 1.497(8) .
C4 C5 1.375(11) .
C4 H4A 0.9500 .
C5 N1 1.308(11) .
C5 H5A 0.9500 .
C6 O3 1.246(8) .
C6 O2 1.266(8) .
C7 N2 1.334(8) .
C7 C8 1.402(10) .
C7 H7B 0.9500 .
C8 C9 1.364(9) .
C8 H8A 0.9500 .
C9 C8 1.364(9) 7_575
C9 C10 1.521(14) .
C10 O4 1.227(8) .
C10 O4 1.227(8) 7_575
C11 N3 1.344(17) .
C11 C12 1.36(2) .
C11 C11 1.90(3) 7_575
C11 H11A 0.9500 .
C11' N3 1.336(15) .
C11' C12' 1.389(18) .
C11' C11' 1.92(3) 7_575
C11' H11B 0.9500 .
C12 C13 1.372(18) .
C12 C12 2.01(3) 7_575
C12 H12A 0.9500 .
C12' C13 1.394(15) .
C12' C12' 2.03(3) 7_575
C12' H12B 0.9500 .
C13 C12 1.372(18) 7_575
C13 C12' 1.394(15) 7_575
C13 C14 1.534(12) .
C14 O5 1.215(7) .
C14 O5 1.215(7) 7_575
N1 Co1 2.192(5) 2_565
N2 C7 1.334(8) 7_575
N2 Co2 2.138(7) 6_656
N3 C11' 1.336(15) 7_575
N3 C11 1.344(17) 7_575
N3 Co2 2.218(8) 1_554
O1 Co1 2.114(3) 7_575
O1 H1B 0.81(10) .
O7 C17 1.4004 7_575
O7 C17 1.4004 .
O7 H7A 0.8499 .
C17 C17 1.1633 7_575
C17 C18 1.525(9) .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C18 C17 1.525(9) 7_575
C18 H18A 0.9600 .
C18 H18B 0.9601 .
C18 H18C 0.9599 .
O6 C15 1.392(9) .
O6 H6A 0.8502 .
C15 C16 1.517(9) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
N4 O8 1.217(9) .
N4 O10 1.223(9) .
N4 O9 1.223(9) .
O10 O10 1.48(6) 5_566
