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_4512530
_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         'C44 H28 Co3 N4 O14'
_chemical_formula_sum            'C44 H28 Co3 N4 O14'
_chemical_formula_weight         1013.49
_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             2014-11-05
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
????
;
_cell_angle_alpha                99.057(11)
_cell_angle_beta                 90.485(9)
_cell_angle_gamma                106.122(10)
_cell_formula_units_Z            2
_cell_length_a                   9.650(6)
_cell_length_b                   17.270(12)
_cell_length_c                   18.274(12)
_cell_measurement_reflns_used    6055
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.2
_cell_volume                     2885(3)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
scan:
    Number of images: 128
               Slice: -110.0000 - 18.0000
         Image width: 1.0000
            Exp time: 30.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -70.0000
                 Phi: 315.0000
                 XTD: 45.2039
              2theta: -20.0967
scan:
    Number of images: 128
               Slice: -110.0000 - 18.0000
         Image width: 1.0000
            Exp time: 30.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -70.0000
                 Phi: 270.0000
                 XTD: 45.2039
              2theta: -20.0967
scan:
    Number of images: 113
               Slice: -110.0000 - 3.0000
         Image width: 1.0000
            Exp time: 30.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -70.0000
                 Phi: 135.0000
                 XTD: 45.2039
              2theta: -20.0967
scan:
    Number of images: 90
               Slice: -87.0000 - 3.0000
         Image width: 1.0000
            Exp time: 30.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 0.0000
                 Phi: 45.0000
                 XTD: 45.2039
              2theta: -20.0967
scan:
    Number of images: 60
               Slice: -110.0000 - -50.0000
         Image width: 1.0000
            Exp time: 30.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 0.0000
                 Phi: 0.0000
                 XTD: 45.2039
              2theta: -20.0967
scan:
    Number of images: 48
               Slice: -86.0000 - -38.0000
         Image width: 1.0000
            Exp time: 30.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -70.0000
                 Phi: 90.0000
                 XTD: 45.2039
              2theta: -20.0967

 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Mitegen
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.105904
_diffrn_orient_matrix_UB_12      0.019681
_diffrn_orient_matrix_UB_13      0.008207
_diffrn_orient_matrix_UB_21      0.015173
_diffrn_orient_matrix_UB_22      0.033514
_diffrn_orient_matrix_UB_23      -0.048816
_diffrn_orient_matrix_UB_31      -0.007945
_diffrn_orient_matrix_UB_32      0.050812
_diffrn_orient_matrix_UB_33      0.020856
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.136
_diffrn_reflns_av_unetI/netI     0.175
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37606
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.515
_diffrn_reflns_theta_min         2.2
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1026
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
The unit cell contains 4 DMF molecules and 5 waters which have been treated 
as a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.744
_refine_diff_density_min         -1.135
_refine_diff_density_rms         0.240
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         13070
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1626
_refine_ls_R_factor_gt           0.0898
_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^)+(0.0985P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2159
_refine_ls_wR_factor_ref         0.2484
_reflns_number_gt                6882
_reflns_number_total             13070
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg501690b_si_003.cif
_cod_data_source_block           am19
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 4512530--4512532.cif.
;
_cod_database_code               4512530
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C3B \\sim C4B \\sim C4B \\sim C5B \\sim C6B: within 1.7A with sigma of 0.008
and sigma for terminal atoms of 0.016
C5C \\sim C6C \\sim C7C \\sim C8C \\sim C3C: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.016
3.a Aromatic/amide H refined with riding coordinates:
 C4C(H4C), C5C(H5C), C7C(H7C), C8C(H8C), C4D(H4D), C5D(H5D), C7D(H7D),
 C8D(H8D), C4F(H4F), C5F(H5F), C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A), C9A(H9A),
  C10A(H10A), C11A(H11A), C12A(H12A), C3B(H3B), C4B(H4B), C5B(H5B), C6B(H6B),
 C9B(H9B), C10B(H10B), C11B(H11B), C12B(H12B), C4E(H4E), C5E(H5E)
;
_olex2_submission_special_instructions 'No special instructions were received'