A Five-Coordinate Heme Dioxygen Adduct Isolated within a Metal-Organic Framework.
Anderson, John S.; Gallagher, Audrey T.; Mason, Jarad A.; Harris, T. David; Journal of the American Chemical Society  (2014) 141117151249006–; doi:10.1021/ja5103103

data_4122995
_publ_section_title
;
 A Five-Coordinate Heme Dioxygen Adduct Isolated within a Metal-Organic
 Framework.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              141117151249006
_journal_paper_doi               10.1021/ja5103103
_journal_year                    2014
_chemical_formula_moiety         '0.25(C576 H288 Fe12 N48 O256 Zr48)'
_chemical_formula_sum            'C144 H72 Fe3 N12 O64 Zr12'
_chemical_formula_weight         4256.32
_chemical_name_systematic
;
 ?
;
_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             2014-10-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
Note that there are several Level A alerts for PCN-224FeO2 (2).  These arise from the short O-O distances in the
bound oxygen unit and are likely an artifact of the disorder of the dioxygen unit around the crystallographic
fourfold axis. One other Level A alert similarly arises from a short O-O distance near the Zr cluster which again 
arises from disorder.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   38.4265(16)
_cell_length_b                   38.4265(16)
_cell_length_c                   38.4265(16)
_cell_measurement_reflns_used    6900
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.06
_cell_measurement_theta_min      2.81
_cell_volume                     56740(4)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.01
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            322200
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.199
_diffrn_reflns_theta_min         1.626
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.553
_exptl_absorpt_correction_T_max  0.3196
_exptl_absorpt_correction_T_min  0.2257
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0578 before and 0.0485 after correction.
The Ratio of minimum to maximum transmission is 0.7062.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    0.498
_exptl_crystal_description       cube
_exptl_crystal_F_000             8360
_refine_diff_density_max         1.176
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         4847
_refine_ls_number_restraints     248
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1740P)^2^+9.9690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2273
_refine_ls_wR_factor_ref         0.2397
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3651
_reflns_number_total             4847
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5103103_si_002.cif
_cod_data_source_block           PCN-224Fe
_cod_original_cell_volume        56740(7)
_cod_database_code               4122995
_shelxl_version_number           2013-4
_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 1.7A 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) O2(0.25) O10(0.5) O12(0.25) O8(0.5) O1(0.5)
 O20(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C23(H23)
;
_shelx_res_checksum              65474
_shelx_hkl_checksum              83951
_olex2_submission_special_instructions 'No special instructions were received'