#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:51:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179309 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/06/4320639.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_4320639
loop_
_publ_author_name
'Yen-Hsiang Liu'
'Hui-Lien Tsai'
'Yi-Long Lu'
'Yuh-Sheng Wen'
'Ju-Chun Wang'
'Kuang-Lieh Lu'
_publ_section_title
;
 Assembly of a Robust, Thermally Stable Porous Cobalt(II) Nicotinate
 Framework Based on a Dicobalt Carboxylate Unit
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6426
_journal_page_last               6431
_journal_paper_doi               10.1021/ic010528k
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C31 H26 Co2 N4 O10'
_chemical_formula_weight         732.42
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2001-05-01T10:33:16-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                106.7180
_cell_angle_beta                 102.2790
_cell_angle_gamma                111.1900
_cell_formula_units_Z            2
_cell_length_a                   10.6671(6)
_cell_length_b                   12.0063(7)
_cell_length_c                   14.0658(8)
_cell_measurement_temperature    298(2)
_cell_volume                     1504.11(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7478
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    1.17
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.698
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'DARK ORANGE'
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.64
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.36
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0087(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         5180
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.504
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0587P)²+1.2491P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1013
_reflns_number_gt                5030
_reflns_number_total             5180
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010528k_3.cif
_cod_data_source_block           conico3
_cod_database_code               4320639
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.19349(3) 0.49579(3) 0.21403(2) 0.02573(12) Uani 1 1 d . . .
Co2 Co 0.54787(3) 0.76829(3) 0.30975(2) 0.02554(12) Uani 1 1 d . . .
N11 N 0.7175(2) 0.7486(2) 0.24944(15) 0.0309(4) Uani 1 1 d . . .
N21 N 0.3351(2) 1.0228(2) 0.63134(16) 0.0310(4) Uani 1 1 d . . .
N31 N 0.1661(2) 0.3467(2) 0.27369(16) 0.0315(4) Uani 1 1 d . . .
N41 N 0.0342(2) 0.5651(2) -0.15862(15) 0.0299(4) Uani 1 1 d . . .
O11 O 0.83667(18) 0.63066(18) -0.06080(13) 0.0352(4) Uani 1 1 d . . .
O12 O 0.60944(19) 0.5754(2) -0.06981(14) 0.0450(5) Uani 1 1 d . . .
O21 O 0.21659(19) 0.61851(16) 0.35963(13) 0.0338(4) Uani 1 1 d . . .
O22 O 0.40297(18) 0.80232(16) 0.38268(13) 0.0346(4) Uani 1 1 d . . .
O31 O 0.3346(2) 0.22509(17) 0.54799(13) 0.0356(4) Uani 1 1 d . . .
O32 O 0.4026(3) 0.4364(2) 0.58297(16) 0.0569(6) Uani 1 1 d . . .
O41 O 0.21720(18) 0.63790(18) 0.15104(14) 0.0337(4) Uani 1 1 d . . .
O42 O 0.44152(17) 0.74653(17) 0.15672(13) 0.0320(4) Uani 1 1 d . . .
O91 O 0.42395(18) 0.56144(17) 0.25822(15) 0.0297(4) Uani 1 1 d . . .
H91 H 0.477(4) 0.554(4) 0.314(3) 0.070(11) Uiso 1 1 d . . .
H92 H 0.425(3) 0.524(3) 0.207(3) 0.039(9) Uiso 1 1 d . . .
C31 C 0.0777(3) 0.2216(3) 0.2109(2) 0.0404(6) Uani 1 1 d . . .
H31A H 0.0254 0.2007 0.141 0.048 Uiso 1 1 calc R . .
C11 C 0.8543(3) 0.7957(3) 0.3129(2) 0.0379(6) Uani 1 1 d . . .
H11A H 0.8777 0.8332 0.3859 0.045 Uiso 1 1 calc R . .
C12 C 0.9616(3) 0.7907(3) 0.2745(2) 0.0441(7) Uani 1 1 d . . .
H12A H 1.0544 0.8224 0.3213 0.053 Uiso 1 1 calc R . .
C13 C 0.9309(3) 0.7387(3) 0.1662(2) 0.0392(6) Uani 1 1 d . . .
H13A H 1.0025 0.7366 0.1389 0.047 Uiso 1 1 calc R . .
C14 C 0.7901(3) 0.6896(2) 0.09950(18) 0.0289(5) Uani 1 1 d . . .
C15 C 0.6883(3) 0.6955(2) 0.14471(18) 0.0300(5) Uani 1 1 d . . .
H15A H 0.5937 0.6604 0.0996 0.036 Uiso 1 1 calc R . .
C16 C 0.7418(3) 0.6278(2) -0.02006(19) 0.0296(5) Uani 1 1 d . . .
C21 C 0.2713(4) 0.9614(3) 0.6864(2) 0.0499(8) Uani 1 1 d . . .
H21A H 0.2713 1.0112 0.7507 0.06 Uiso 1 1 calc R . .
C22 C 0.2054(5) 0.8273(3) 0.6516(3) 0.0683(11) Uani 1 1 d . . .
H22A H 0.1599 0.7881 0.6911 0.082 Uiso 1 1 calc R . .
C23 C 0.2079(4) 0.7523(3) 0.5577(3) 0.0525(8) Uani 1 1 d . . .
H23A H 0.1634 0.6618 0.5328 0.063 Uiso 1 1 calc R . .
C24 C 0.2776(3) 0.8136(2) 0.50112(19) 0.0316(5) Uani 1 1 d . . .
C25 C 0.3369(2) 0.9485(2) 0.54031(18) 0.0290(5) Uani 1 1 d . . .
H25A H 0.3805 0.99 0.5012 0.035 Uiso 1 1 calc R . .
C26 C 0.3002(2) 0.7387(2) 0.40570(18) 0.0279(5) Uani 1 1 d . . .
C35 C 0.2416(3) 0.3752(2) 0.37441(19) 0.0331(5) Uani 1 1 d . . .
H35A H 0.3023 0.4621 0.4193 0.04 Uiso 1 1 calc R . .
C32 C 0.0604(3) 0.1221(3) 0.2449(2) 0.0489(7) Uani 1 1 d . . .
H32A H -0.0034 0.0362 0.1992 0.059 Uiso 1 1 calc R . .
C33 C 0.1393(3) 0.1521(3) 0.3477(2) 0.0435(6) Uani 1 1 d . . .
H33A H 0.1297 0.0864 0.3723 0.052 Uiso 1 1 calc R . .
C34 C 0.2326(3) 0.2804(3) 0.4142(2) 0.0346(5) Uani 1 1 d . . .
C36 C 0.3308(3) 0.3180(3) 0.52440(19) 0.0347(5) Uani 1 1 d . . .
C41 C 0.1120(3) 0.5602(3) -0.2215(2) 0.0424(6) Uani 1 1 d . . .
H41A H 0.0667 0.5333 -0.294 0.051 Uiso 1 1 calc R . .
C42 C 0.2561(3) 0.5932(4) -0.1835(2) 0.0555(9) Uani 1 1 d . . .
H42A H 0.3062 0.5865 -0.2299 0.067 Uiso 1 1 calc R . .
C43 C 0.3261(3) 0.6370(3) -0.0747(2) 0.0451(7) Uani 1 1 d . . .
H43A H 0.424 0.6623 -0.047 0.054 Uiso 1 1 calc R . .
C44 C 0.2469(2) 0.6422(2) -0.00881(18) 0.0289(5) Uani 1 1 d . . .
C45 C 0.1016(3) 0.6037(2) -0.05472(19) 0.0288(5) Uani 1 1 d . . .
H45A H 0.0477 0.6049 -0.0108 0.035 Uiso 1 1 calc R . .
C46 C 0.3070(2) 0.6786(2) 0.10914(18) 0.0279(5) Uani 1 1 d . . .
C91 C 0.3334(6) 1.0761(4) 0.1048(4) 0.0898(14) Uani 1 1 d . . .
C92 C 0.4037(4) 1.2003(4) 0.1836(4) 0.0747(11) Uani 1 1 d . A .
H92A H 0.4234 1.2713 0.1648 0.09 Uiso 1 1 calc R . .
C93 C 0.4458(4) 1.2220(4) 0.2900(4) 0.0748(11) Uani 1 1 d . . .
H93A H 0.4968 1.3063 0.3423 0.09 Uiso 1 1 calc R A .
C94 C 0.4095(5) 1.1138(5) 0.3167(4) 0.0787(12) Uani 1 1 d . A .
H94A H 0.4359 1.1275 0.3881 0.094 Uiso 1 1 calc R . .
C95 C 0.3367(5) 0.9888(4) 0.2417(4) 0.0797(12) Uani 1 1 d . . .
H95A H 0.3124 0.918 0.2608 0.096 Uiso 1 1 calc R A .
C96 C 0.3001(6) 0.9714(4) 0.1349(4) 0.1025(18) Uani 1 1 d . A .
H96A H 0.2521 0.8871 0.0824 0.123 Uiso 1 1 calc R . .
C97A C 0.310(4) 1.063(3) -0.025(2) 0.164(11) Uani 0.5 1 d P A 1
C97B C 0.276(4) 1.058(2) -0.0025(16) 0.133(12) Uani 0.5 1 d P A 2
O92A O 0.4584(15) 1.0500(14) -0.0456(11) 0.199(6) Uani 0.5 1 d P A 1
O92B O 0.2670(8) 0.9471(8) -0.0749(5) 0.107(2) Uani 0.5 1 d P A 2
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 0 '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 0.006 '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
_geom_angle_publ_flag
O21 Co1 O41 92.90(7) . . ?
O21 Co1 O11 178.06(7) . 2_665 ?
O41 Co1 O11 86.13(7) . 2_665 ?
O21 Co1 N31 88.62(7) . . ?
O41 Co1 N31 178.35(7) . . ?
O11 Co1 N31 92.32(8) 2_665 . ?
O21 Co1 N41 90.69(7) . 2_565 ?
O41 Co1 N41 87.78(7) . 2_565 ?
O11 Co1 N41 87.59(7) 2_665 2_565 ?
N31 Co1 N41 91.57(8) . 2_565 ?
O21 Co1 O91 92.19(7) . . ?
O41 Co1 O91 88.08(7) . . ?
O11 Co1 O91 89.47(7) 2_665 . ?
N31 Co1 O91 92.50(7) . . ?
N41 Co1 O91 175.07(7) 2_565 . ?
O31 Co2 O42 172.36(7) 2_666 . ?
O31 Co2 O22 88.30(7) 2_666 . ?
O42 Co2 O22 98.65(7) . . ?
O31 Co2 O91 89.23(7) 2_666 . ?
O42 Co2 O91 87.55(7) . . ?
O22 Co2 O91 90.49(7) . . ?
O31 Co2 N21 89.56(7) 2_666 2_676 ?
O42 Co2 N21 94.08(7) . 2_676 ?
O22 Co2 N21 85.92(7) . 2_676 ?
O91 Co2 N21 176.25(7) . 2_676 ?
O31 Co2 N11 87.27(7) 2_666 . ?
O42 Co2 N11 86.02(7) . . ?
O22 Co2 N11 173.97(7) . . ?
O91 Co2 N11 93.53(7) . . ?
N21 Co2 N11 89.96(8) 2_676 . ?
C15 N11 C11 116.7(2) . . ?
C15 N11 Co2 119.99(16) . . ?
C11 N11 Co2 123.12(16) . . ?
C21 N21 C25 117.3(2) . . ?
C21 N21 Co2 123.08(17) . 2_676 ?
C25 N21 Co2 119.31(16) . 2_676 ?
C31 N31 C35 117.8(2) . . ?
C31 N31 Co1 121.03(16) . . ?
C35 N31 Co1 121.12(17) . . ?
C45 N41 C41 117.5(2) . . ?
C45 N41 Co1 117.80(16) . 2_565 ?
C41 N41 Co1 124.59(17) . 2_565 ?
C16 O11 Co1 127.02(15) . 2_665 ?
C26 O21 Co1 126.12(15) . . ?
C26 O22 Co2 138.07(16) . . ?
C36 O31 Co2 129.02(16) . 2_666 ?
C46 O41 Co1 127.11(15) . . ?
C46 O42 Co2 122.72(15) . . ?
Co2 O91 Co1 114.16(8) . . ?
N31 C31 C32 123.0(2) . . ?
N11 C11 C12 122.9(2) . . ?
C11 C12 C13 119.8(2) . . ?
C12 C13 C14 118.0(2) . . ?
C15 C14 C13 118.4(2) . . ?
C15 C14 C16 118.3(2) . . ?
C13 C14 C16 123.3(2) . . ?
N11 C15 C14 124.0(2) . . ?
O12 C16 O11 125.7(2) . . ?
O12 C16 C14 116.4(2) . . ?
O11 C16 C14 117.8(2) . . ?
N21 C21 C22 122.8(3) . . ?
C23 C22 C21 119.3(3) . . ?
C22 C23 C24 119.1(3) . . ?
C23 C24 C25 117.7(2) . . ?
C23 C24 C26 121.6(2) . . ?
C25 C24 C26 120.5(2) . . ?
N21 C25 C24 123.8(2) . . ?
O22 C26 O21 127.1(2) . . ?
O22 C26 C24 116.4(2) . . ?
O21 C26 C24 116.4(2) . . ?
N31 C35 C34 122.8(2) . . ?
C33 C32 C31 118.8(3) . . ?
C32 C33 C34 119.5(2) . . ?
C33 C34 C35 118.1(2) . . ?
C33 C34 C36 121.9(2) . . ?
C35 C34 C36 119.9(2) . . ?
O32 C36 O31 125.9(2) . . ?
O32 C36 C34 118.0(2) . . ?
O31 C36 C34 116.0(2) . . ?
N41 C41 C42 122.8(2) . . ?
C41 C42 C43 119.1(3) . . ?
C44 C43 C42 118.6(2) . . ?
C43 C44 C45 118.0(2) . . ?
C43 C44 C46 124.0(2) . . ?
C45 C44 C46 117.9(2) . . ?
N41 C45 C44 123.8(2) . . ?
O41 C46 O42 125.9(2) . . ?
O41 C46 C44 116.1(2) . . ?
O42 C46 C44 118.1(2) . . ?
C92 C91 C96 118.1(4) . . ?
C92 C91 C97B 119.6(9) . . ?
C96 C91 C97B 121.4(10) . . ?
C92 C91 C97A 116.7(11) . . ?
C96 C91 C97A 124.8(12) . . ?
C97B C91 C97A 15(2) . . ?
C91 C92 C93 121.7(4) . . ?
C92 C93 C94 118.3(4) . . ?
C95 C94 C93 122.3(4) . . ?
C94 C95 C96 117.5(4) . . ?
C91 C96 C95 122.0(4) . . ?
O92A C97A C91 103.8(18) . . ?
O92B C97B C91 113.5(14) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O21 2.0525(17) . ?
Co1 O41 2.1007(17) . ?
Co1 O11 2.1268(17) 2_665 ?
Co1 N31 2.142(2) . ?
Co1 N41 2.150(2) 2_565 ?
Co1 O91 2.1722(17) . ?
Co2 O31 2.0861(17) 2_666 ?
Co2 O42 2.1005(16) . ?
Co2 O22 2.1208(17) . ?
Co2 O91 2.1504(18) . ?
Co2 N21 2.154(2) 2_676 ?
Co2 N11 2.213(2) . ?
N11 C15 1.340(3) . ?
N11 C11 1.344(3) . ?
N21 C21 1.340(3) . ?
N21 C25 1.342(3) . ?
N21 Co2 2.154(2) 2_676 ?
N31 C31 1.335(3) . ?
N31 C35 1.345(3) . ?
N41 C45 1.338(3) . ?
N41 C41 1.339(3) . ?
N41 Co1 2.150(2) 2_565 ?
O11 C16 1.259(3) . ?
O11 Co1 2.1268(17) 2_665 ?
O12 C16 1.250(3) . ?
O21 C26 1.258(3) . ?
O22 C26 1.257(3) . ?
O31 C36 1.264(3) . ?
O31 Co2 2.0861(17) 2_666 ?
O32 C36 1.247(3) . ?
O41 C46 1.253(3) . ?
O42 C46 1.267(3) . ?
C31 C32 1.377(4) . ?
C11 C12 1.378(4) . ?
C12 C13 1.382(4) . ?
C13 C14 1.388(3) . ?
C14 C15 1.383(3) . ?
C14 C16 1.510(3) . ?
C21 C22 1.381(4) . ?
C22 C23 1.380(4) . ?
C23 C24 1.387(4) . ?
C24 C25 1.388(3) . ?
C24 C26 1.506(3) . ?
C35 C34 1.388(4) . ?
C32 C33 1.376(4) . ?
C33 C34 1.380(4) . ?
C34 C36 1.506(3) . ?
C41 C42 1.376(4) . ?
C42 C43 1.394(4) . ?
C43 C44 1.384(4) . ?
C44 C45 1.385(3) . ?
C44 C46 1.511(3) . ?
C91 C92 1.379(6) . ?
C91 C96 1.391(6) . ?
C91 C97B 1.421(18) . ?
C91 C97A 1.75(2) . ?
C92 C93 1.383(6) . ?
C93 C94 1.399(6) . ?
C94 C95 1.366(6) . ?
C95 C96 1.402(6) . ?
C97A O92A 1.72(4) . ?
C97B O92B 1.38(3) . ?
