Dioxygen binding at a four-coordinate cobaltous porphyrin site in a metal‒organic framework: structural, EPR, and O2 adsorption analysis
Gallagher, Audrey T.; Kelty, Margaret L.; Park, Jesse G.; Anderson, John S.; Mason, Jarad A.; Walsh, James P. S.; Collins, Shenell L.; Harris, T. David; Inorganic Chemistry Frontiers 3 (2016) 536–; doi:10.1039/C5QI00275C

data_4349086
_publ_section_title
;
 Dioxygen binding at a four-coordinate cobaltous porphyrin site in a
 metal--organic framework: structural, EPR, and O2 adsorption analysis
;
_journal_issue                   4
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              536
_journal_paper_doi               10.1039/C5QI00275C
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety         '0.25(C576 H288 Co12 N48 O280 Zr48)'
_chemical_formula_sum            'C144 H72 Co3 N12 O70 Zr12'
_chemical_formula_weight         4361.56
_chemical_name_systematic        PCN224CoO2
_space_group_crystal_system      cubic
_space_group_IT_number           229
_space_group_name_Hall           '-I 4 2 3'
_space_group_name_H-M_alt        'I m -3 m'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/cc1kl9ct
_audit_creation_date             2016-01-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-01-15 deposited with the CCDC.
2016-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   38.6198(10)
_cell_length_b                   38.6198(10)
_cell_length_c                   38.6198(10)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      65.20
_cell_measurement_theta_min      6.68
_cell_volume                     57601(3)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      84.83
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1022
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            93162
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        65.616
_diffrn_reflns_theta_max         65.616
_diffrn_reflns_theta_min         5.842
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.598
_exptl_absorpt_correction_T_max  .374
_exptl_absorpt_correction_T_min  .313
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.503
_exptl_crystal_description       cube
_exptl_crystal_F_000             8564
_exptl_crystal_size_max          0.508
_exptl_crystal_size_mid          0.417
_exptl_crystal_size_min          0.379
_refine_diff_density_max         2.207
_refine_diff_density_min         -1.075
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.329
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         4619
_refine_ls_number_restraints     233
_refine_ls_restrained_S_all      1.347
_refine_ls_R_factor_all          0.1102
_refine_ls_R_factor_gt           0.0988
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2976
_refine_ls_wR_factor_ref         0.3131
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3584
_reflns_number_total             4619
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00275c2.cif
_cod_data_source_block           PCN224CoO2
_cod_original_cell_volume        57601(4)
_cod_database_code               4349086
_shelx_estimated_absorpt_t_max   0.439
_shelx_estimated_absorpt_t_min   0.352
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.1 and sigma
for terminal atoms of 0.2
4. Others
 Fixed Sof: Zr1(0.25) Zr2(0.25) Co1(0.125) O1(0.125) O2(0.125)
5.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C3(H3), C4(H4)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'