#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:51:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179309 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/06/4320637.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_4320637
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_compound_source        'synthesis as described'
_chemical_formula_moiety         'C12 H8 Co1 O4'
_chemical_formula_structural     'C12 H8 CO1 O4'
_chemical_formula_sum            'C25 H22 Co2 N4 O10'
_chemical_formula_weight         656.33
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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/cifdics/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2001-05-01T00:39:58-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                106.878(4)
_cell_angle_beta                 102.411(2)
_cell_angle_gamma                111.011(3)
_cell_formula_units_Z            2
_cell_length_a                   10.5407(2)
_cell_length_b                   11.8266(3)
_cell_length_c                   14.1122(2)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     1467.89(9)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
   x-axis points to radiation source
   the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.13117E-1
_diffrn_orient_matrix_UB_12      0.62805E-1
_diffrn_orient_matrix_UB_13      -0.35783E-1
_diffrn_orient_matrix_UB_21      -0.107814
_diffrn_orient_matrix_UB_22      -0.33198E-1
_diffrn_orient_matrix_UB_23      -0.29043E-1
_diffrn_orient_matrix_UB_31      0.00649
_diffrn_orient_matrix_UB_32      0.68908E-1
_diffrn_orient_matrix_UB_33      0.64507E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.011
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5465
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.61
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.189
_exptl_absorpt_correction_T_max  0.7786
_exptl_absorpt_correction_T_min  0.6192
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
         Number of psi-scan sets used was   5
         Theta correction was applied.
         Weighted transmission curves were used.
         No Fourier smoothing was applied.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       0.0037(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         5155
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0739P)²+1.8118P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1145
_reflns_number_gt                4268
_reflns_number_total             5155
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010528k_1.cif
_cod_data_source_block           conico1
_cod_original_cell_volume        1467.89(5)
_cod_database_code               4320637
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 0.19330(4) 0.49141(4) 0.21267(3) 0.02621(14) Uani 1 1 d . . .
Co2 Co 0.54880(4) 0.76918(4) 0.30993(3) 0.02628(14) Uani 1 1 d . . .
N11 N 0.7186(3) 0.7471(3) 0.25007(19) 0.0313(6) Uani 1 1 d . . .
N21 N 0.3352(3) 1.0188(2) 0.63313(19) 0.0320(6) Uani 1 1 d . . .
N31 N 0.1675(3) 0.3376(3) 0.2683(2) 0.0337(6) Uani 1 1 d . . .
N41 N 0.0366(3) 0.5703(2) -0.15750(19) 0.0296(5) Uani 1 1 d . . .
O11 O 0.8370(2) 0.6353(2) -0.06026(16) 0.0373(5) Uani 1 1 d . . .
O12 O 0.6096(3) 0.5867(3) -0.07013(19) 0.0606(8) Uani 1 1 d . . .
O21 O 0.2173(2) 0.6124(2) 0.35927(16) 0.0338(5) Uani 1 1 d . . .
O22 O 0.3998(2) 0.7999(2) 0.38042(17) 0.0378(5) Uani 1 1 d . . .
O31 O 0.3335(3) 0.2169(2) 0.54515(16) 0.0388(5) Uani 1 1 d . . .
O32 O 0.4040(3) 0.4298(3) 0.5765(2) 0.0609(8) Uani 1 1 d . . .
O41 O 0.2148(2) 0.6349(2) 0.14962(17) 0.0349(5) Uani 1 1 d . . .
O42 O 0.4414(2) 0.7516(2) 0.16033(16) 0.0331(5) Uani 1 1 d . . .
C11 C 0.8546(4) 0.7874(3) 0.3126(2) 0.0377(7) Uani 1 1 d . . .
H11A H 0.878 0.8221 0.3857 0.045 Uiso 1 1 calc R . .
C12 C 0.9620(4) 0.7797(4) 0.2734(3) 0.0425(8) Uani 1 1 d . . .
H12A H 1.0546 0.8062 0.3195 0.051 Uiso 1 1 calc R . .
C13 C 0.9308(3) 0.7326(3) 0.1655(3) 0.0363(7) Uani 1 1 d . . .
H13A H 1.0025 0.7293 0.1377 0.044 Uiso 1 1 calc R . .
C14 C 0.7906(3) 0.6904(3) 0.0994(2) 0.0302(6) Uani 1 1 d . . .
C15 C 0.6884(3) 0.6981(3) 0.1454(2) 0.0321(7) Uani 1 1 d . . .
H15A H 0.5934 0.6673 0.1008 0.039 Uiso 1 1 calc R . .
C16 C 0.7421(3) 0.6338(3) -0.0199(2) 0.0316(7) Uani 1 1 d . . .
C21 C 0.2690(5) 0.9563(4) 0.6860(3) 0.0578(11) Uani 1 1 d . . .
H21B H 0.2674 1.006 0.7499 0.069 Uiso 1 1 calc R . .
C22 C 0.2027(7) 0.8204(4) 0.6495(4) 0.091(2) Uani 1 1 d . . .
H22A H 0.1536 0.7796 0.6869 0.109 Uiso 1 1 calc R . .
C23 C 0.2093(6) 0.7455(4) 0.5579(4) 0.0661(13) Uani 1 1 d . . .
H23A H 0.1665 0.6537 0.5332 0.079 Uiso 1 1 calc R . .
C24 C 0.2805(3) 0.8085(3) 0.5032(2) 0.0333(7) Uani 1 1 d . . .
C25 C 0.3394(3) 0.9451(3) 0.5433(2) 0.0290(6) Uani 1 1 d . . .
H25A H 0.3846 0.988 0.5053 0.035 Uiso 1 1 calc R . .
C26 C 0.3011(3) 0.7342(3) 0.4059(2) 0.0282(6) Uani 1 1 d . . .
C31 C 0.0784(4) 0.2109(3) 0.2051(3) 0.0450(9) Uani 1 1 d . . .
H31A H 0.0238 0.19 0.1358 0.054 Uiso 1 1 calc R . .
C32 C 0.0638(5) 0.1095(4) 0.2383(3) 0.0611(12) Uani 1 1 d . . .
H32A H -0.001 0.0224 0.1925 0.073 Uiso 1 1 calc R . .
C33 C 0.1462(4) 0.1390(4) 0.3400(3) 0.0523(10) Uani 1 1 d . . .
H33A H 0.1398 0.0721 0.3635 0.063 Uiso 1 1 calc R . .
C34 C 0.2386(3) 0.2699(3) 0.4065(2) 0.0353(7) Uani 1 1 d . . .
C35 C 0.2452(3) 0.3656(3) 0.3679(2) 0.0343(7) Uani 1 1 d . . .
H35A H 0.3066 0.4537 0.4131 0.041 Uiso 1 1 calc R . .
C36 C 0.3336(4) 0.3096(3) 0.5191(2) 0.0363(7) Uani 1 1 d . . .
C41 C 0.1186(4) 0.5697(4) -0.2184(3) 0.0409(8) Uani 1 1 d . . .
H41B H 0.0745 0.5423 -0.291 0.049 Uiso 1 1 calc R . .
C42 C 0.2645(4) 0.6080(4) -0.1776(3) 0.0517(10) Uani 1 1 d . . .
H42A H 0.3176 0.6054 -0.2223 0.062 Uiso 1 1 calc R . .
C43 C 0.3330(4) 0.6509(4) -0.0692(3) 0.0432(8) Uani 1 1 d . . .
H43A H 0.4327 0.6798 -0.0401 0.052 Uiso 1 1 calc R . .
C44 C 0.2495(3) 0.6495(3) -0.0057(2) 0.0288(6) Uani 1 1 d . . .
C45 C 0.1022(3) 0.6071(3) -0.0543(2) 0.0292(6) Uani 1 1 d . . .
H45A H 0.0454 0.604 -0.0121 0.035 Uiso 1 1 calc R . .
C46 C 0.3065(3) 0.6818(3) 0.1109(2) 0.0278(6) Uani 1 1 d . . .
O91 O 0.4260(2) 0.5586(2) 0.25748(17) 0.0305(5) Uani 1 1 d . . .
H91 H 0.4186 0.5186 0.2116 0.042(13) Uiso 1 1 d R . .
H92 H 0.4735 0.5517 0.31 0.054(12) Uiso 1 1 d R . .
C91 C 0.280(4) 0.048(3) 0.051(3) 0.227(13) Uiso 0.5 1 d P . .
C92 C 0.303(3) 0.015(3) -0.024(3) 0.222(12) Uiso 0.5 1 d P . .
O92 O 0.383(3) 0.043(2) 0.127(2) 0.289(11) Uiso 0.5 1 d P . .
O93 O 0.316(3) -0.033(2) 0.2693(19) 0.304(11) Uiso 0.5 1 d P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Co Co 0.3494 0.9721 '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'
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'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-4 1 2
-4 0 2
-5 3 0
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 94.38(9) . . ?
O21 Co1 O11 178.61(8) . 2_665 ?
O41 Co1 O11 85.72(9) . 2_665 ?
O21 Co1 N31 88.66(9) . . ?
O41 Co1 N31 176.90(9) . . ?
O11 Co1 N31 91.22(10) 2_665 . ?
O21 Co1 N41 91.01(9) . 2_565 ?
O41 Co1 N41 87.35(9) . 2_565 ?
O11 Co1 N41 87.62(9) 2_665 2_565 ?
N31 Co1 N41 91.99(10) . 2_565 ?
O21 Co1 O91 91.67(9) . . ?
O41 Co1 O91 88.52(8) . . ?
O11 Co1 O91 89.71(8) 2_665 . ?
N31 Co1 O91 92.01(9) . . ?
N41 Co1 O91 175.24(9) 2_565 . ?
O31 Co2 O42 175.86(9) 2_666 . ?
O31 Co2 O22 86.87(9) 2_666 . ?
O42 Co2 O22 97.25(9) . . ?
O31 Co2 O91 90.84(9) 2_666 . ?
O42 Co2 O91 88.73(8) . . ?
O22 Co2 O91 90.23(8) . . ?
O31 Co2 N21 88.62(9) 2_666 2_676 ?
O42 Co2 N21 92.00(9) . 2_676 ?
O22 Co2 N21 86.92(9) . 2_676 ?
O91 Co2 N21 177.13(9) . 2_676 ?
O31 Co2 N11 88.83(9) 2_666 . ?
O42 Co2 N11 87.07(9) . . ?
O22 Co2 N11 175.09(9) . . ?
O91 Co2 N11 92.20(9) . . ?
N21 Co2 N11 90.61(10) 2_676 . ?
C11 N11 C15 117.2(3) . . ?
C11 N11 Co2 123.7(2) . . ?
C15 N11 Co2 119.01(19) . . ?
C21 N21 C25 117.5(3) . . ?
C21 N21 Co2 124.1(2) . 2_676 ?
C25 N21 Co2 118.2(2) . 2_676 ?
C31 N31 C35 117.7(3) . . ?
C31 N31 Co1 121.7(2) . . ?
C35 N31 Co1 120.6(2) . . ?
C45 N41 C41 117.3(3) . . ?
C45 N41 Co1 116.80(19) . 2_565 ?
C41 N41 Co1 125.8(2) . 2_565 ?
C16 O11 Co1 127.4(2) . 2_665 ?
C26 O21 Co1 125.56(19) . . ?
C26 O22 Co2 137.3(2) . . ?
C36 O31 Co2 127.7(2) . 2_666 ?
C46 O41 Co1 128.7(2) . . ?
C46 O42 Co2 123.52(19) . . ?
N11 C11 C12 122.8(3) . . ?
C13 C12 C11 119.5(3) . . ?
C12 C13 C14 118.4(3) . . ?
C13 C14 C15 118.2(3) . . ?
C13 C14 C16 123.5(3) . . ?
C15 C14 C16 118.3(3) . . ?
N11 C15 C14 123.7(3) . . ?
O12 C16 O11 125.4(3) . . ?
O12 C16 C14 116.9(3) . . ?
O11 C16 C14 117.7(3) . . ?
N21 C21 C22 122.3(3) . . ?
C23 C22 C21 119.8(4) . . ?
C22 C23 C24 118.8(4) . . ?
C23 C24 C25 117.6(3) . . ?
C23 C24 C26 122.2(3) . . ?
C25 C24 C26 120.1(3) . . ?
N21 C25 C24 123.9(3) . . ?
O22 C26 O21 127.0(3) . . ?
O22 C26 C24 116.7(3) . . ?
O21 C26 C24 116.3(3) . . ?
N31 C31 C32 122.7(3) . . ?
C33 C32 C31 119.1(3) . . ?
C32 C33 C34 118.8(3) . . ?
C35 C34 C33 118.5(3) . . ?
C35 C34 C36 119.8(3) . . ?
C33 C34 C36 121.7(3) . . ?
N31 C35 C34 123.1(3) . . ?
O32 C36 O31 126.3(3) . . ?
O32 C36 C34 117.5(3) . . ?
O31 C36 C34 116.2(3) . . ?
N41 C41 C42 122.5(3) . . ?
C41 C42 C43 119.7(3) . . ?
C44 C43 C42 118.5(3) . . ?
C43 C44 C45 117.7(3) . . ?
C43 C44 C46 124.2(3) . . ?
C45 C44 C46 118.0(3) . . ?
N41 C45 C44 124.3(3) . . ?
O41 C46 O42 126.0(3) . . ?
O41 C46 C44 116.4(3) . . ?
O42 C46 C44 117.6(3) . . ?
Co2 O91 Co1 113.64(9) . . ?
C92 C91 O92 104(4) . . ?
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 2.046(2) . ?
Co1 O41 2.100(2) . ?
Co1 O11 2.113(2) 2_665 ?
Co1 N31 2.137(3) . ?
Co1 N41 2.145(2) 2_565 ?
Co1 O91 2.166(2) . ?
Co2 O31 2.077(2) 2_666 ?
Co2 O42 2.081(2) . ?
Co2 O22 2.112(2) . ?
Co2 O91 2.152(2) . ?
Co2 N21 2.153(3) 2_676 ?
Co2 N11 2.201(2) . ?
N11 C11 1.335(4) . ?
N11 C15 1.337(4) . ?
N21 C21 1.328(4) . ?
N21 C25 1.334(4) . ?
N21 Co2 2.153(3) 2_676 ?
N31 C31 1.333(4) . ?
N31 C35 1.340(4) . ?
N41 C45 1.331(4) . ?
N41 C41 1.343(4) . ?
N41 Co1 2.145(2) 2_565 ?
O11 C16 1.250(4) . ?
O11 Co1 2.113(2) 2_665 ?
O12 C16 1.245(4) . ?
O21 C26 1.255(4) . ?
O22 C26 1.249(4) . ?
O31 C36 1.254(4) . ?
O31 Co2 2.077(2) 2_666 ?
O32 C36 1.243(4) . ?
O41 C46 1.248(4) . ?
O42 C46 1.260(4) . ?
C11 C12 1.382(5) . ?
C12 C13 1.378(5) . ?
C13 C14 1.383(4) . ?
C14 C15 1.388(4) . ?
C14 C16 1.509(4) . ?
C21 C22 1.377(6) . ?
C22 C23 1.370(6) . ?
C23 C24 1.378(5) . ?
C24 C25 1.383(4) . ?
C24 C26 1.507(4) . ?
C31 C32 1.381(5) . ?
C32 C33 1.375(5) . ?
C33 C34 1.381(5) . ?
C34 C35 1.379(5) . ?
C34 C36 1.513(4) . ?
C41 C42 1.367(5) . ?
C42 C43 1.389(5) . ?
C43 C44 1.384(4) . ?
C44 C45 1.384(4) . ?
C44 C46 1.504(4) . ?
C91 C92 1.13(4) . ?
C91 O92 1.38(3) . ?
