Hemicubane topological analogs of the oxygen-evolving complex of photosystem II mediating water-assisted propylene carbonate oxidation
Koellner, Connor A.; Gau, Michael; Polyak, Aleksander; Bayana, Manish; Zdilla, Michael John; Chemical Communications  (2022) –; doi:10.1039/D1CC05825H

data_7129561
_publ_section_title
;
 Hemicubane topological analogs of the oxygen-evolving complex of
 photosystem II mediating water-assisted propylene carbonate oxidation
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05825H
_journal_year                    2022
_chemical_formula_moiety         'C24 H36 Mn2 N4 O3 Si2, 0.5(C4 H8 O)'
_chemical_formula_sum            'C26 H40 Mn2 N4 O3.5 Si2'
_chemical_formula_weight         630.68
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-09-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-18 deposited with the CCDC.	2022-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.358(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.028(5)
_cell_length_b                   11.850(4)
_cell_length_c                   20.643(7)
_cell_measurement_reflns_used    3020
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.029
_cell_measurement_theta_min      2.490
_cell_volume                     3181(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'COSMO (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.02
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEX II Duo'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0845
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5414
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         1.566
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0818 before and 0.0674 after correction.
The Ratio of minimum to maximum transmission is 0.8583.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.919
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         5414
_refine_ls_number_restraints     166
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.1057
_refine_ls_R_factor_gt           0.0725
_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^)+(0.0899P)^2^+10.9131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1853
_refine_ls_wR_factor_ref         0.2042
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3860
_reflns_number_total             5414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05825h2.cif
_cod_data_source_block           1
_cod_original_formula_sum        'C26 H40 Mn2 N4 O3.50 Si2'
_cod_database_code               7129561
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.799
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.850(4)
 0.150(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C3S-C2S = C4S-C2S = C3S-C1S
 1.54 with sigma of 0.005
 C3T-C2T = C4T-C2T = C3T-C1T
 1.54 with sigma of 0.005
 O1S-C4S = O1S-C1S
 1.45 with sigma of 0.005
 O1T-C4T = O1T-C1T
 1.45 with sigma of 0.005
 C4S-C1S
 2.29 with sigma of 0.01
 C4T-C1T
 2.29 with sigma of 0.01
 O1S-C2S = O1S-C3S
 2.44 with sigma of 0.01
 O1T-C2T = O1T-C3T
 2.44 with sigma of 0.01
 C4S-C3S = C1S-C2S
 2.51 with sigma of 0.01
 C4T-C3T = C1T-C2T
 2.51 with sigma of 0.01
4. Rigid bond restraints
 O1S, O1S, C1S, C1S, C2S, C2S, C3S, C3S, C4S, C4S, O1T, O1T, C1T, C1T, C2T,
 C2T, C3T, C3T, C4T, C4T
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O1S \\sim O1S \\sim C1S \\sim C1S \\sim C2S \\sim C2S \\sim C3S \\sim C3S \\sim
C4S \\sim C4S \\sim O1T \\sim O1T \\sim C1T \\sim C1T \\sim C2T \\sim C2T \\sim
C3T \\sim C3T \\sim C4T \\sim C4T: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
6. Others
 Sof(O1T)=Sof(C1T)=Sof(H1TA)=Sof(H1TB)=Sof(C2T)=Sof(H2TA)=Sof(H2TB)=Sof(C3T)=
 Sof(H3TA)=Sof(H3TB)=Sof(C4T)=Sof(H4TA)=Sof(H4TB)=0.5*(1-FVAR(2))
 Sof(O1S)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(C3S)=
 Sof(H3SA)=Sof(H3SB)=Sof(C4S)=Sof(H4SA)=Sof(H4SB)=0.5*FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B), C1S(H1SA,H1SB), C2S(H2SA,H2SB),
 C3S(H3SA,H3SB), C4S(H4SA,H4SB), C1T(H1TA,H1TB), C2T(H2TA,H2TB), C3T(H3TA,H3TB),
  C4T(H4TA,H4TB)
7.b Me refined with riding coordinates:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
7.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16)
;
_shelx_res_checksum              10896
_olex2_submission_special_instructions 'No special instructions were received'