Enhancing catalytic alkane hydroxylation by tuning the outer coordination sphere in a heme-containing metal-organic framework.
Zee, David Z.; Harris, T. David; Chemical science 11 (2020) 5447–5452; doi:10.1039/d0sc01796e

data_1558029
_publ_section_title
;
 Enhancing catalytic alkane hydroxylation by tuning the outer coordination
 sphere in a heme-containing metal-organic framework.
;
_journal_issue                   21
_journal_name_full               'Chemical science'
_journal_page_first              5447
_journal_page_last               5452
_journal_paper_doi               10.1039/d0sc01796e
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C168 H108 Cl3 Fe3 N12 O64 Zr12'
_chemical_formula_sum            'C168 H108 Cl3 Fe3 N12 O64 Zr12'
_chemical_formula_weight         4687.20
_chemical_melting_point          ?
_chemical_name_common            PCN-224'FeCl
_chemical_name_systematic        '[FeCl(TCPP)]3[ZrO4(OH)4(CH3CO2)6]2'
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2020-02-24
_audit_creation_method
;
Olex2 1.3
(compiled 2019.11.21 svn.r41b79517 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-03-26 deposited with the CCDC.	2020-05-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   38.4891(9)
_cell_length_b                   38.4891(9)
_cell_length_c                   38.4891(9)
_cell_measurement_reflns_used    9484
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      63.721
_cell_measurement_theta_min      3.631
_cell_volume                     57018(2)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2017)'
_computing_data_collection       'APEX2 V2017.3 (Bruker, 2017)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0524
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            167138
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        63.832
_diffrn_reflns_theta_max         63.832
_diffrn_reflns_theta_min         3.248
_diffrn_source                   microsource
_diffrn_source_current           0.64
_diffrn_source_power             0.0286336
_diffrn_source_voltage           44.74
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.687
_exptl_absorpt_correction_T_max  0.7524
_exptl_absorpt_correction_T_min  0.6566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0422 before and 0.0334 after correction.
The Ratio of minimum to maximum transmission is 0.8727.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    0.546
_exptl_crystal_description       cuboctahedral
_exptl_crystal_F_000             9284
_exptl_crystal_recrystallization_method
'See Experimental Section in Supporting Information'
_exptl_crystal_size_max          0.248
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.219
_refine_diff_density_max         0.937
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         4417
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0733
_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^)+(0.1299P)^2^+126.4133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2249
_refine_ls_wR_factor_ref         0.2456
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3868
_reflns_number_total             4417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01796e2.cif
_cod_data_source_block           PCN-224'FeCl
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 1558028--1558030.cif.

 Adding full bibliography for 1558028--1558030.cif.
;
_cod_original_cell_volume        57018(4)
_cod_database_code               1558029
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.591
_shelx_estimated_absorpt_t_min   0.555
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C10-C9 \\sim C10A-C9A
 with sigma of 0.02
 C10A-O4 \\sim O4A-C10
 with sigma of 0.04
 C9-O4 \\sim O4A-C9A
 with sigma of 0.02
3. Restrained planarity
 O4, O4_$2, C9, C10
 with sigma of 0.1
 O4A_$1, O4A, C9A, C10A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 0.9A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 0.9A
Uanis(C10) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 Zr1, O1, O2, O4, C9, C10, O2A, O4A, C9A, C10A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Fe1, Cl1, O3, N1, C1, C2, C3, C4, C5, C6, C7, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O4A)=1-FVAR(1)
 Sof(C9A)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=0.5*(1-FVAR(2))
 Sof(C9)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=0.5*FVAR(2)
 Sof(O4)=FVAR(1)
 Sof(O2A)=0.5*(1-FVAR(3))
 Sof(O2)=0.5*FVAR(3)
 Fixed Sof: Fe1(0.125) Cl1(0.125)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C8(H8)
7.b Idealised Me refined with riding coordinates:
 C10(H10A,H10B,H10C), C10A(H10D,H10E,H10F)
;
_shelx_res_checksum              5449
_olex2_exptl_crystal_mounting_method
; 
In a solvent-free, dinitrogen-filled glovebox, activated crystals were coated 
with Paratone-N oil. The crystals were removed from the glovebox. A suitable 
single crystal was mounted on a MiTeGen loop, and cooled under a stream of N2 
at 100 K for collection.
;
_olex2_submission_original_sample_id PCN-224'FeCl
_olex2_submission_special_instructions 'No special instructions were received'