Reactive Pendant Mn═O in a Synthetic Structural Model of a Proposed S4 State in the Photosynthetic Oxygen Evolving Complex.
Vaddypally, Shivaiah; Kondaveeti, Sandeep K.; Karki, Santosh; Van Vliet, Megan M.; Levis, Robert J.; Zdilla, Michael J.; Journal of the American Chemical Society 139 (2017) 4675–4681; doi:10.1021/jacs.6b05906

data_4126155
_publ_section_title
;
 Reactive Pendant Mn&#x2550;O in a Synthetic Structural Model of a
 Proposed S4 State in the Photosynthetic Oxygen Evolving Complex.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4675
_journal_page_last               4681
_journal_paper_doi               10.1021/jacs.6b05906
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C28 H64 Mn4 N8'
_chemical_formula_sum            'C28 H64 Mn4 N8'
_chemical_formula_weight         732.63
_space_group_crystal_system      trigonal
_space_group_IT_number           160
_space_group_name_Hall           'R 3 -2"'
_space_group_name_H-M_alt        'R 3 m :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-04-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   34.7647(11)
_cell_length_b                   34.7647(11)
_cell_length_c                   10.8425(4)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.895
_cell_measurement_theta_min      2.344
_cell_volume                     11348.5(7)
_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      99.95
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker KAPPA APEX II DUO'
_diffrn_measurement_method       '\f, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            36362
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.895
_diffrn_reflns_theta_min         1.996
_exptl_absorpt_coefficient_mu    1.332
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0494 before and 0.0419 after correction.
The Ratio of minimum to maximum transmission is 0.9058.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       bar
_exptl_crystal_F_000             4656
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 2781 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         6147
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0215
_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^)+(0.0324P)^2^+8.4721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0543
_refine_ls_wR_factor_ref         0.0551
_reflns_Friedel_coverage         0.936
_reflns_Friedel_fraction_full    0.968
_reflns_Friedel_fraction_max     0.942
_reflns_number_gt                5929
_reflns_number_total             6147
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b05906_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-07-04
;
_cod_original_cell_volume        11348.5(8)
_cod_database_code               4126155
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.675
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All N(H) groups
2. Restrained distances
 C90-C93
 1.54 with sigma of 0.004
 C80-C83 = C80-C81 = C80-C82
 1.54 with sigma of 0.001
 C6-C61 = C6-C62 = C6-C63 = C6-C61A = C6-C62A = C6-C63A
 1.54 with sigma of 0.004
 C93-C91 = C91-C92 = C92-C93
 2.52 with sigma of 0.008
 C83-C81 = C81-C82 = C82-C83
 2.52 with sigma of 0.002
 N8-C83 = N8-C81 = N8-C82
 2.44 with sigma of 0.002
 C61-C62 = C62-C63 = C63-C61
 2.52 with sigma of 0.008
 C61A-C62A = C62A-C63A = C63A-C61A
 2.52 with sigma of 0.008
 N6-C61 = N6-C62 = N6-C63 = N6-C61A = N6-C62A = N6-C62A
 2.44 with sigma of 0.008
3. Rigid bond restraints
 C6, C61, C61A, C62, C62A, C63, C63A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
C6 \\sim C61 \\sim C61A \\sim C62 \\sim C62A \\sim C63 \\sim C63A: within 1.7A
with sigma of 0.002 and sigma for terminal atoms of 0.004
5. Others
 Sof(C61A)=Sof(H61D)=Sof(H61E)=Sof(H61F)=Sof(C62A)=Sof(H62D)=Sof(H62E)=
 Sof(H62F)=Sof(C63A)=Sof(H63D)=Sof(H63E)=Sof(H63F)=1-FVAR(1)
 Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(H61C)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=
 Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=FVAR(1)
 Fixed Sof: H32B(0.5) H32C(0.5) C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5)
 C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5) C43(0.5) H43A(0.5) H43B(0.5) H43C(0.5)
 C51(0.5) H51A(0.5) H51B(0.5) H51C(0.5) Mn5(0.5) N8(0.5) N9(0.5) C80(0.5)
 C81(0.5) H81A(0.5) H81B(0.5) H81C(0.5) C82(0.5) H82A(0.5) H82B(0.5) H82C(0.5)
 C83(0.5) H83A(0.5) H83B(0.5) H83C(0.5) C90(0.5) C91(0.5) H91A(0.5) H91B(0.5)
 H91C(0.5) C92(0.5) H92A(0.5) H92B(0.5) H92C(0.5) C93(0.5) H93A(0.5) H93B(0.5)
 H93C(0.5) C101(0.5) H10A(0.5) H10B(0.5) H10C(0.5)
6.a Me refined with riding coordinates:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C61(H61A,H61B,H61C),
 C61A(H61D,H61E,H61F), C62(H62A,H62B,H62C), C62A(H62D,H62E,H62F), C63(H63A,H63B,
 H63C), C63A(H63D,H63E,H63F), C81(H81A,H81B,H81C), C82(H82A,H82B,H82C),
 C83(H83A,H83B,H83C), C101(H10A,H10B,H10C)
6.b Idealised Me refined as rotating group:
 C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C)
;
_shelx_res_checksum              16059
_shelx_hkl_checksum              23828
_olex2_submission_special_instructions 'No special instructions were received'