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_4130449
_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         '(C100 H76 Cl3 Co12 N80 O12) Co1.5'
_chemical_formula_sum            'C100 H76 Cl3 Co13.5 N80 O12'
_chemical_formula_weight         3492.20
_chemical_name_common            Co-BDTriP-MeOH
_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             2016-02-04
_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                   18.7059(4)
_cell_length_b                   18.7059(4)
_cell_length_c                   18.7059(4)
_cell_measurement_reflns_used    9578
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.07
_cell_measurement_theta_min      2.43
_cell_volume                     6545.4(2)
_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 7.9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       '\w/\q scans'
_diffrn_radiation_monochromator  'QUAZAR multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0867
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            55966
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.100
_diffrn_reflns_theta_max         24.100
_diffrn_reflns_theta_min         1.089
_diffrn_source                   'microfocus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.906
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1210 before and 0.0806 after correction.
The Ratio of minimum to maximum transmission is 0.9369.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    0.864
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1707
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.405
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         1108
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0974P)^2^+18.7104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.1761
_reflns_Friedel_coverage         0.000
_reflns_number_gt                974
_reflns_number_total             1108
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b03680_si_001.cif
_cod_data_source_block           Co-BDTriP-MeOH
_cod_original_cell_volume        6545.4(4)
_cod_database_code               4130449
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.938
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups
2. Shared sites
{N2, C1}
3. Uiso/Uaniso restraints and constraints
O1 \\sim C5: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C1) = Uanis(N2)
4. Rigid body (RIGU) restrains
 O1, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N2(0.667) C1(0.333) H1(0.333) C5(0.25) H5F(0.125) H5C(0.125)
 H5D(0.125) H5B(0.125) H5E(0.125) H5A(0.125)
6.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C1(H1)
6.b Disordered Me refined with riding coordinates:
 C5(H5F,H5C,H5D,H5B,H5E,H5A)
;
_shelx_res_checksum              86994
_shelx_hkl_checksum              26020
_shelx_fab_checksum              91352
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'