Tetranuclear [Mn<sup>III</sup>Mn<sub>3</sub><sup>IV</sup>O<sub>4</sub>] Complexes as Spectroscopic Models of the S<sub>2</sub> State of the Oxygen Evolving Complex in Photosystem II.
Lee, Heui Beom; Shiau, Angela A.; Oyala, Paul H.; Marchiori, David A.; Gul, Sheraz; Chatterjee, Ruchira; Yano, Junko; Britt, R. David; Agapie, Theodor; Journal of the American Chemical Society 140 (2018) 17175–17187; doi:10.1021/jacs.8b09961

data_4133421
_publ_section_title
;
 Tetranuclear [Mn<sup>III</sup>Mn<sub>3</sub><sup>IV</sup>O<sub>4</sub>]
 Complexes as Spectroscopic Models of the S<sub>2</sub> State of the
 Oxygen Evolving Complex in Photosystem II.
;
_journal_issue                   49
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17175
_journal_page_last               17187
_journal_paper_doi               10.1021/jacs.8b09961
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C72 H55 F3 Mn4 N8 O11, C F3 O3 S, C4 H10 O'
_chemical_formula_sum            'C77 H65 F6 Mn4 N8 O15 S'
_chemical_formula_weight         1708.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-07-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 122.4230(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   41.9795(15)
_cell_length_b                   15.5642(8)
_cell_length_c                   26.7105(8)
_cell_measurement_reflns_used    9625
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.62
_cell_volume                     14731.5(10)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       59
_diffrn_reflns_limit_h_min       -59
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            150607
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.561
_diffrn_reflns_theta_min         2.164
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7016
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0673 before and 0.0493 after correction.
The Ratio of minimum to maximum transmission is 0.9404.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       block
_exptl_crystal_F_000             6984
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.7016
_refine_diff_density_max         2.579
_refine_diff_density_min         -2.608
_refine_diff_density_rms         0.247
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1004
_refine_ls_number_reflns         22494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0766
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1552P)^2^+65.4176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2334
_refine_ls_wR_factor_ref         0.2585
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17368
_reflns_number_total             22494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09961_si_002.cif
_cod_data_source_block           4-ox
_cod_database_code               4133421
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.925
_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.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C6(H6A,H6B), C75(H75A,H75B), C76(H76A,H76B)
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C73(H73), C69(H69), C31(H31), C60(H60), C66(H66), C38(H38),
 C41(H41), C51(H51), C20(H20), C54(H54), C42(H42), C37(H37), C71(H71), C40(H40),
  C52(H52), C18(H18), C28(H28), C57(H57), C36(H36), C35(H35), C65(H65),
 C39(H39), C63(H63), C29(H29), C53(H53), C30(H30), C19(H19), C64(H64), C46(H46),
  C58(H58), C27(H27), C59(H59), C49(H49), C24(H24), C26(H26), C25(H25),
 C14(H14), C48(H48), C47(H47), C13(H13), C11(H11), C10(H10)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C74(H74A,H74B,H74C), C77(H77A,H77B,H77C)
;
_shelx_res_checksum              95444
_shelx_hkl_checksum              6212
_shelx_fab_checksum              15141
_olex2_submission_special_instructions 'No special instructions were received'