CO Binding at a Four-Coordinate Cobaltous Porphyrin Site in a Metal-Organic Framework: Structural, EPR, and Gas Adsorption Analysis.
Gallagher, Audrey T.; Malliakas, Christos D.; Harris, T. David; Inorganic chemistry 56 (2017) 4655–4662; doi:10.1021/acs.inorgchem.7b00292

data_4345636
_publ_section_title
;
 CO Binding at a Four-Coordinate Cobaltous Porphyrin Site in a
 Metal-Organic Framework: Structural, EPR, and Gas Adsorption Analysis.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4655
_journal_page_last               4662
_journal_paper_doi               10.1021/acs.inorgchem.7b00292
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         '0.25(C587.61 H288 Co12 N48 O267.61 Zr48)'
_chemical_formula_sum            'C146.9 H72 Co3 N12 O66.9 Zr12'
_chemical_formula_weight         4346.86
_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'
_symmetry_space_group_name_Hall  '-I 4 2 3'
_symmetry_space_group_name_H-M   'I m -3 m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-01-13
_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            4
_cell_length_a                   38.4988(8)
_cell_length_b                   38.4988(8)
_cell_length_c                   38.4988(8)
_cell_measurement_reflns_used    7883
_cell_measurement_temperature    200
_cell_measurement_theta_max      61.389
_cell_measurement_theta_min      2.812
_cell_volume                     57061(2)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_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)'
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'QuazarTM optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1630
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            141824
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        61.385
_diffrn_reflns_theta_max         61.385
_diffrn_reflns_theta_min         2.295
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.618
_exptl_absorpt_correction_T_max  0.3189
_exptl_absorpt_correction_T_min  0.1875
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1779 before and 0.0742 after correction. The Ratio of minimum to maximum transmission is 0.5880. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.506
_exptl_crystal_description       cube
_exptl_crystal_F_000             8535
_exptl_crystal_size_max          0.392
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.224
_refine_diff_density_max         2.051
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.288
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         4147
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.377
_refine_ls_R_factor_all          0.1203
_refine_ls_R_factor_gt           0.1013
_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          0.2959
_refine_ls_wR_factor_ref         0.3145
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3007
_reflns_number_total             4147
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00292_si_005.cif
_cod_data_source_block           PCN224CoCO_200K
_cod_depositor_comments
'Adding full bibliography for 4345635--4345637.cif.'
_cod_original_cell_volume        57061(4)
_cod_original_formula_sum        'C146.90 H72 Co3 N12 O66.90 Zr12'
_cod_database_code               4345636
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O5-C9
 1.18 with sigma of 0.02
3. 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
4. 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
Uanis(Zr2) = Uanis(Zr1)
Uanis(O1) = Uanis(O3)
5. Others
 Sof(Zr2)=0.5*(1-FVAR(2))
 Sof(Zr1)=0.5*FVAR(2)
 Fixed Sof: C9(0.12095) O5(0.12095)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6), C5(H5)
;
_shelx_res_checksum              34113
_shelx_hkl_checksum              77421
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'