Selective, Tunable O2 Binding in Cobalt(II)-Triazolate/Pyrazolate Metal-Organic Frameworks.
Xiao, Dianne J.; Gonzalez, Miguel I.; Darago, Lucy E.; Vogiatzis, Konstantinos D.; Haldoupis, Emmanuel; Gagliardi, Laura; Long, Jeffrey R.; Journal of the American Chemical Society 138 (2016) 7161–7170; doi:10.1021/jacs.6b03680

data_4130448
_publ_section_title
;
 Selective, Tunable O2 Binding in Cobalt(II)-Triazolate/Pyrazolate
 Metal-Organic Frameworks.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7161
_journal_page_last               7170
_journal_paper_doi               10.1021/jacs.6b03680
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         '(C140 H140 Cl3 Co12 N76 O12) Co1.4 O1.4'
_chemical_formula_sum            'C140 H140 Cl3 Co14.4 N76 O14.4'
_chemical_formula_weight         4072.57
_chemical_name_common            Co-BDTriP-DMF
_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_Hall           '-P 4 2 3'
_space_group_name_H-M_alt        'P m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-02-03
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   18.8345(7)
_cell_length_b                   18.8345(7)
_cell_length_c                   18.8345(7)
_cell_measurement_reflns_used    9810
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.174
_cell_measurement_theta_min      2.636
_cell_volume                     6681.3(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker PHOTON100 CMOS diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'channel-cut Si(111) crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_unetI/netI     0.0122
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            97274
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         30.174
_diffrn_reflns_theta_min         2.358
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.949
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1253 before and 0.0670 after correction.
The Ratio of minimum to maximum transmission is 0.9275.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.012
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1683
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         1577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0916P)^2^+6.3029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1590
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1404
_reflns_number_total             1577
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b03680_si_001.cif
_cod_data_source_block           Co-BDTriP-DMF
_cod_original_cell_volume        6681.3(7)
_cod_original_formula_sum        'C140 H140 Cl3 Co14.40 N76 O14.40'
_cod_database_code               4130448
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.911
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{N2, C1}
3. Uiso/Uaniso restraints and constraints
Co2 \\sim O2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(N2) = Uanis(C1)
4. Others
 Fixed Sof: C1(0.6667) H1(0.6667) Co2(0.05) O2(0.05) N2(0.3333)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C1(H1)
;
_shelx_res_checksum              50397
_shelx_hkl_checksum              35674
_shelx_fab_checksum              95493
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'