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_4345784
_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(C599.33 H288 Co12 N48 O279.33 Zr48)'
_chemical_formula_sum            'C149.83 H72 Co3 N12 O69.83 Zr12'
_chemical_formula_weight         4428.93
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-13
_audit_creation_method
;
Olex2 1.2
(compiled Dec 12 2016 15:38:10 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   38.5333(8)
_cell_length_b                   38.5333(8)
_cell_length_c                   38.5333(8)
_cell_measurement_reflns_used    9824
_cell_measurement_temperature    80
_cell_measurement_theta_max      67.10
_cell_measurement_theta_min      6.70
_cell_volume                     57215(2)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      80
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0824
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            83768
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.285
_diffrn_reflns_theta_max         67.285
_diffrn_reflns_theta_min         6.699
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.619
_exptl_absorpt_correction_T_max  0.3114
_exptl_absorpt_correction_T_min  0.1789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1036 before and 0.0717 after correction.
The Ratio of minimum to maximum transmission is 0.5745.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.514
_exptl_crystal_description       cube
_exptl_crystal_F_000             8699
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.208
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.177
_refine_diff_density_min         -1.444
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.463
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         4702
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.551
_refine_ls_R_factor_all          0.1258
_refine_ls_R_factor_gt           0.1112
_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          0.3293
_refine_ls_wR_factor_ref         0.3490
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3681
_reflns_number_total             4702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00292_si_003.cif
_cod_data_source_block           PCN224CoCO_80K
_cod_original_cell_volume        57215(4)
_cod_database_code               4345784
_shelx_shelxl_version_number     2014/7
_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(0.24299) O5(0.24299)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6), C5(H5)
;
_olex2_submission_special_instructions 'No special instructions were received'