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_4512531
_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         'C26 H16 Co2 N2 O10, 0.75(O), 1.25(C O)'
_chemical_formula_sum            'C27.25 H22.5 Co2 N2 O12'
_chemical_formula_weight         687.83
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_date             2014-08-08
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                88.868(6)
_cell_angle_beta                 69.339(5)
_cell_angle_gamma                85.726(5)
_cell_formula_units_Z            2
_cell_length_a                   11.3407(5)
_cell_length_b                   11.3847(9)
_cell_length_c                   13.1908(7)
_cell_measurement_reflns_used    2913
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.3577
_cell_measurement_theta_min      2.9633
_cell_volume                     1589.07(18)
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.2833
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_details
;
  1 omega   -6.00   98.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       16.3155   19.0000    0.0000 104

  2 omega   -7.00   90.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       16.3155   38.0000   90.0000 97

  3 omega   40.00  106.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       16.3155  178.0000  -60.0000 66

  4 omega -107.00  -82.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.2530 -178.0000 -180.0000 25

  5 omega -104.00  -57.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.2530 -178.0000    0.0000 47

  6 omega  -18.00   25.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.2530  -99.0000  120.0000 43
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0665043000
_diffrn_orient_matrix_UB_12      -0.0072260000
_diffrn_orient_matrix_UB_13      0.0235144000
_diffrn_orient_matrix_UB_21      -0.0132079000
_diffrn_orient_matrix_UB_22      0.0569202000
_diffrn_orient_matrix_UB_23      -0.0195140000
_diffrn_orient_matrix_UB_31      0.0015857000
_diffrn_orient_matrix_UB_32      -0.0265272000
_diffrn_orient_matrix_UB_33      -0.0493411000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1120
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13478
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.091
_diffrn_reflns_theta_min         2.944
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.105
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85991
_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    1.438
_exptl_crystal_description       block
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.070
_refine_diff_density_min         -1.318
_refine_diff_density_rms         0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         13478
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1518
_refine_ls_R_factor_gt           0.1072
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1950P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2674
_refine_ls_wR_factor_ref         0.2947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8854
_reflns_number_total             13478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg501690b_si_002.cif
_cod_data_source_block           am31
_cod_depositor_comments
'Adding full bibliography for 4512530--4512532.cif.'
_cod_original_formula_sum        'C27.25 H22.50 Co2 N2 O12'
_cod_database_code               4512531
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C20 H20 N2 O2 Co'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C36-O36
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C5 \\sim C17 \\sim C19: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C8 \\sim C12: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C21 \\sim C22 \\sim C23 \\sim C24: within 1.7A with sigma of 0.008 and sigma
for terminal atoms of 0.016
Co1 \\sim Co3 \\sim O14 \\sim N13: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008
O14 \\sim O15 \\sim O16 \\sim O20 \\sim O21 \\sim O25 \\sim O26 \\sim O30 \\sim
O31: within 1.7A with sigma of 0.008 and sigma for terminal atoms of 0.08
O36 \\sim C36: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C18 \\sim C26 \\sim C27 \\sim C28: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C12) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C27) \\sim Ueq:
with sigma of 0.008 and sigma for terminal atoms of 0.016
Uanis(O1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O31) \\sim Ueq:
with sigma of 0.002 and sigma for terminal atoms of 0.004
4. Others
 Fixed Sof: O35(0.5) O35A(0.5) C35A(0.5) O36(0.5) C36(0.5) O36A(0.25)
 C36A(0.25) O37(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C18(H18), C19(H19), C23(H23), C24(H24), C28(H28), C29(H29), C33(H33), C34(H34)
;
_olex2_exptl_crystal_mounting_method 'crystal mounted with fromblin'
_olex2_submission_special_instructions 'No special instructions were received'