A structurally-characterized peroxomanganese(iv) porphyrin from reversible O<sub>2</sub> binding within a metal-organic framework.
Gallagher, Audrey T.; Lee, Jung Yoon; Kathiresan, Venkatesan; Anderson, John S.; Hoffman, Brian M.; Harris, T. David; Chemical science 9 (2018) 1596–1603; doi:10.1039/c7sc03739b

data_1548466
_publ_section_title
;
 A structurally-characterized peroxomanganese(iv) porphyrin from
 reversible O<sub>2</sub> binding within a metal-organic framework.
;
_journal_issue                   6
_journal_name_full               'Chemical science'
_journal_page_first              1596
_journal_page_last               1603
_journal_paper_doi               10.1039/c7sc03739b
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         '0.25(C576 H288 Mn12 N48 O208 Zr48)'
_chemical_formula_sum            'C144 H72 Mn3 N12 O52 Zr12'
_chemical_formula_weight         4061.59
_chemical_name_systematic        PCN224Mn
_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             2017-06-20
_audit_creation_method
;
Olex2 1.2
(compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-08-23 deposited with the CCDC.
2017-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   38.6720(10)
_cell_length_b                   38.6720(10)
_cell_length_c                   38.6720(10)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    100
_cell_measurement_theta_max      64.91
_cell_measurement_theta_min      2.28
_cell_volume                     57835(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0934
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            154240
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.349
_diffrn_reflns_theta_min         2.285
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.409
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6302
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0825 before and 0.0713 after correction.
The Ratio of minimum to maximum transmission is 0.8368.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    0.466
_exptl_crystal_description       Cube
_exptl_crystal_F_000             7964
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.489
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         4950
_refine_ls_number_restraints     211
_refine_ls_restrained_S_all      1.237
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0844
_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^)+(0.1790P)^2^+83.5939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2432
_refine_ls_wR_factor_ref         0.2639
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4013
_reflns_number_total             4950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03739b2.cif
_cod_data_source_block           PCN224Mn
_cod_depositor_comments
'Adding full bibliography for 1548465--1548466.cif.'
_cod_original_cell_volume        57835(4)
_cod_database_code               1548466
_shelx_shelxl_version_number     2014/7
_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
Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(Zr1) \\sim
Ueq, Uanis(Zr2) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4)
\\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq,
Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N17) \\sim
Ueq, : with sigma of 0.03 and sigma for terminal atoms of 0.06
Uanis(Mn1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(Zr1)=0.5*(1-FVAR(2))
 Sof(Zr2)=0.5*FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C6(H6)
;
_shelx_res_checksum              13569
_shelx_fab_checksum              14519
_olex2_submission_original_sample_id PCN224Mn
_olex2_submission_special_instructions 'No special instructions were received'