Metal‒Organic Frameworks from Divalent Metals and 1,4-Benzenedicarboxylate with Bidentate Pyridine-N-oxide Co-ligands
Munn, Alexis S.; Amabilino, Silvia; Stevens, Thomas W.; Daniels, Luke M.; Clarkson, Guy J.; Millange, Franck; Lennox, Matthew J.; Düren, Tina; Bourelly, Sandrine; Llewellyn, Philip L.; Walton, Richard I.; Crystal Growth & Design 15 (2015) 891–; doi:10.1021/cg501690b

data_4512532
_publ_section_title
;
 Metal--Organic Frameworks from Divalent Metals and
 1,4-Benzenedicarboxylate with Bidentate Pyridine-N-oxide Co-ligands
;
_journal_issue                   2
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              891
_journal_paper_doi               10.1021/cg501690b
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         '0.5(C52 H32 Co4 N4 O20)'
_chemical_formula_sum            'C26 H16 Co2 N2 O10'
_chemical_formula_weight         634.27
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-05-06
_audit_creation_method
;
  Olex2 1.2
  (compiled 2013.04.25 svn.r2679, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 110.274(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.3517(12)
_cell_length_b                   11.3956(10)
_cell_length_c                   13.2806(12)
_cell_measurement_reflns_used    1323
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      30.1873
_cell_measurement_theta_min      2.9046
_cell_volume                     1611.5(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 10.2833
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details
;
  1 omega   68.00  114.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8608  178.0000   90.0000 46

  2 omega    8.00  110.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8608    3.0000   34.0000 102

  3 omega  -74.00  -45.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8608    3.0000   34.0000 29

  4 omega  -99.00  -65.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6421 -178.0000  -30.0000 34

  5 omega   -6.00   27.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6421  -99.0000   90.0000 33

  6 omega  -18.00  103.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8608   38.0000  150.0000 121

  7 omega  -18.00  103.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8608   38.0000  -90.0000 121

  8 omega -116.00  -57.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6421 -178.0000   90.0000 59

  9 omega  -87.00  -58.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.6421  135.0000  -10.0000 29
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0421250000
_diffrn_orient_matrix_UB_12      0.0459850000
_diffrn_orient_matrix_UB_13      -0.0006108000
_diffrn_orient_matrix_UB_21      -0.0456082000
_diffrn_orient_matrix_UB_22      0.0421944000
_diffrn_orient_matrix_UB_23      0.0012675000
_diffrn_orient_matrix_UB_31      0.0244915000
_diffrn_orient_matrix_UB_32      -0.0004424000
_diffrn_orient_matrix_UB_33      0.0569978000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_unetI/netI     0.1754
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13810
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.283
_diffrn_reflns_theta_min         3.165
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.079
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.815
_refine_diff_density_min         -1.527
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         13810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.1554
_refine_ls_R_factor_gt           0.0738
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0419P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1261
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7630
_reflns_number_total             13810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg501690b_si_001.cif
_cod_data_source_block           am33
_cod_depositor_comments
'Adding full bibliography for 4512530--4512532.cif.'
_cod_database_code               4512532
_chemical_oxdiff_formula         'C20 H20 N2 O2 Co'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C16(H16), C17(H17)
;
_shelxl_version_number           2013-2