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_7129562
_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         'C52 H80 Ca Mn3 N8 O7 Si4, C4 H8 O'
_chemical_formula_sum            'C56 H88 Ca Mn3 N8 O8 Si4'
_chemical_formula_weight         1318.60
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                 93.239(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5216(15)
_cell_length_b                   19.661(3)
_cell_length_c                   32.220(5)
_cell_measurement_reflns_used    9667
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      2.74
_cell_volume                     6654.5(17)
_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      100.06
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            110437
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.971
_diffrn_reflns_theta_min         2.736
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0630 before and 0.0408 after correction.
The Ratio of minimum to maximum transmission is 0.9222.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_description       block
_exptl_crystal_F_000             2780
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.061
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     779
_refine_ls_number_reflns         15931
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+6.7010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0848
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13967
_reflns_number_total             15931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05825h2.cif
_cod_data_source_block           2
_cod_original_cell_volume        6654.7(17)
_cod_database_code               7129562
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.750
_shelx_estimated_absorpt_t_min   0.679
_olex2_refinement_description
;
1. 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
2. Restrained distances
 C2T-C1T = O1S-C1S = O1T-C1T = C4T-O1T = C4S-O1S = C2S-C3S = C2T-C3T = C3S-C4S
 = C3T-C4T = C2S-C1S
 1.5 with sigma of 0.005
 O1S-C1S = O1S-C4S = O1T-C1T = O1T-C4T
 1.45 with sigma of 0.02
 C2S-C1S = C3S-C2S = C4S-C3S = C2T-C1T = C3T-C2T = C4T-C3T
 1.54 with sigma of 0.02
 O1T-C2T = O1S-C2S = C1T-C4T = C1T-C3T = C1S-C4S = C1S-C3S = O1T-C3T = C2T-C4T
 = C2S-C4S = O1S-C3S
 2.4 with sigma of 0.01
 C1S-C4S
 2.29 with sigma of 0.04
 C1T-C4T
 2.29 with sigma of 0.04
 O1S-C2S
 2.44 with sigma of 0.04
 O1S-C3S
 2.44 with sigma of 0.04
 O1T-C2T
 2.44 with sigma of 0.04
 O1T-C3T
 2.44 with sigma of 0.04
 C1S-C3S
 2.51 with sigma of 0.04
 C4S-C2S
 2.51 with sigma of 0.04
 C1T-C3T
 2.51 with sigma of 0.04
 C2T-C4T
 2.51 with sigma of 0.04
3. Rigid bond restraints
 O1S, C1S, C2S, C3S, C4S, O1T, C1T, C2T, C3T, C4T
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O1S \\sim C1S \\sim C2S \\sim C3S \\sim C4S \\sim O1T \\sim C1T \\sim C2T \\sim
C3T \\sim C4T: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Others
 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)=1-FVAR(1)
 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)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C0AA(H0AA,H0AB), C6(H6A,H6B), C12(H12A,H12B), C24(H24B,H24A), C30(H30A,H30B),
 C36(H36A,H36B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B),
  C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C1T(H1TA,
 H1TB), C2T(H2TA,H2TB), C3T(H3TA,H3TB), C4T(H4TA,H4TB)
6.b 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), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25),
  C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33), C34(H34)
6.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C)
;
_shelx_res_checksum              59063
_olex2_submission_special_instructions 'No special instructions were received'