Synthesis and Characterization of Symmetrically versus Unsymmetrically Proton-Bridged Hexa-Iron Clusters
De Silva, D. Nirosha T.; Dais, Tyson N.; Jameson, Geoffrey B.; Cutler, Daniel J.; Brechin, Euan K.; Davies, Casey G.; Jameson, Guy N. L.; Plieger, Paul G.; ACS Omega 6 (2021) 16661–16669; doi:10.1021/acsomega.1c02255

data_4518819
_publ_section_title
;
 Synthesis and Characterization of Symmetrically versus Unsymmetrically
 Proton-Bridged Hexa-Iron Clusters
;
_journal_issue                   25
_journal_name_full               'ACS Omega'
_journal_page_first              16661
_journal_page_last               16669
_journal_paper_doi               10.1021/acsomega.1c02255
_journal_volume                  6
_journal_year                    2021
_chemical_formula_moiety         'C111 H126 F6 Fe6 N12 O14, C5 H5 N, 3(B F4)'
_chemical_formula_sum            'C116 H131 B3 F18 Fe6 N13 O14'
_chemical_formula_weight         2640.86
_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
_audit_creation_date             2020-12-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.409(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9936(4)
_cell_length_b                   37.0613(7)
_cell_length_c                   20.4370(14)
_cell_measurement_reflns_used    20812
_cell_measurement_temperature    163
_cell_measurement_theta_max      71.9
_cell_measurement_theta_min      6.6
_cell_volume                     12507.0(12)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 rc14 (Rigaku, 2009)
;
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      163.0
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support Loop
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1969
_diffrn_reflns_av_unetI/netI     0.2057
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            130760
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        65.084
_diffrn_reflns_theta_max         65.084
_diffrn_reflns_theta_min         6.546
_exptl_absorpt_coefficient_mu    6.208
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   EMPIRICAL
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       block
_exptl_crystal_F_000             5452
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1565
_refine_ls_number_reflns         21266
_refine_ls_number_restraints     1090
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.1894
_refine_ls_R_factor_gt           0.1012
_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^)+(0.1358P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2518
_refine_ls_wR_factor_ref         0.3043
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8435
_reflns_number_total             21266
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao1c02255_si_002.cif
_cod_data_source_block           nir-001
_cod_depositor_comments
'Adding full bibliography for 4518818--4518819.cif.'
_cod_database_code               4518819
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.437
_shelx_estimated_absorpt_t_min   0.167
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B1-F1 = B1-F2 = B1-F3 = B1-F4
 1.32715 with sigma of 0.02
 B2A-F5A = B2A-F6A = B2A-F7A = B2A-F8A
 1.32715 with sigma of 0.02
 B2B-F5B = B2B-F6B = B2B-F7B = B2B-F8B
 1.32715 with sigma of 0.02
 B3-F9 = B3-F10 = B3-F11 = B3-F12
 1.32715 with sigma of 0.02
 F1-F2 = F1-F3 = F1-F4 = F2-F3 = F2-F4 = F3-F4
 2.167236 with sigma of 0.02
 F5A-F6A = F5A-F7A = F5A-F8A = F6A-F7A = F6A-F8A = F7A-F8A
 2.167236 with sigma of 0.02
 F5B-F6B = F5B-F7B = F5B-F8B = F6B-F7B = F6B-F8B = F7B-F8B
 2.167236 with sigma of 0.02
 F9-F10 = F9-F11 = F9-F12 = F10-F11 = F10-F12 = F11-F12
 2.167236 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F15 \\sim F16 \\sim F17 \\sim F18 \\sim F19 \\sim F20 \\sim F1 \\sim F2 \\sim
F3 \\sim F4 \\sim F5A \\sim F6A \\sim F7A \\sim F8A \\sim F5B \\sim F6B \\sim
F7B \\sim F8B \\sim F9 \\sim F10 \\sim F11 \\sim F12: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 1.1 within 1.7A
Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C21) \\sim Ueq,
Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq,
Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq,
Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46)
\\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq,
Uanis(C54) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C61)
\\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq,
Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C221) \\sim Ueq, Uanis(C231)
\\sim Ueq, Uanis(C241) \\sim Ueq, Uanis(C251) \\sim Ueq, Uanis(C261) \\sim Ueq,
Uanis(C411) \\sim Ueq, Uanis(C421) \\sim Ueq, Uanis(C431) \\sim Ueq,
Uanis(C441) \\sim Ueq, Uanis(C451) \\sim Ueq, Uanis(C461) \\sim Ueq,
Uanis(C611) \\sim Ueq, Uanis(C613) \\sim Ueq, Uanis(C614) \\sim Ueq,
Uanis(C615) \\sim Ueq, Uanis(C616) \\sim Ueq, Uanis(C617) \\sim Ueq,
Uanis(C618) \\sim Ueq, Uanis(C619) \\sim Ueq, Uanis(C620) \\sim Ueq,
Uanis(C621) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C622) \\sim Ueq, Uanis(C623)
\\sim Ueq, Uanis(C624) \\sim Ueq, Uanis(C625) \\sim Ueq, Uanis(C626) \\sim Ueq,
Uanis(C627) \\sim Ueq, Uanis(C628) \\sim Ueq, Uanis(C629) \\sim Ueq,
Uanis(C630) \\sim Ueq, Uanis(C631) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C633)
\\sim Ueq, Uanis(C634) \\sim Ueq, Uanis(C635) \\sim Ueq, Uanis(C636) \\sim Ueq,
Uanis(C637) \\sim Ueq, Uanis(C638) \\sim Ueq, Uanis(C639) \\sim Ueq,
Uanis(C640) \\sim Ueq, Uanis(C641) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C643)
\\sim Ueq, Uanis(C644) \\sim Ueq, Uanis(C645) \\sim Ueq, Uanis(C646) \\sim Ueq,
Uanis(C647) \\sim Ueq, Uanis(C648) \\sim Ueq, Uanis(C649) \\sim Ueq,
Uanis(C650) \\sim Ueq, Uanis(C651) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C652)
\\sim Ueq, Uanis(C653) \\sim Ueq, Uanis(C654) \\sim Ueq, Uanis(C655) \\sim Ueq,
Uanis(C656) \\sim Ueq, Uanis(C657) \\sim Ueq, Uanis(C658) \\sim Ueq,
Uanis(C659) \\sim Ueq, Uanis(C660) \\sim Ueq, Uanis(C661) \\sim Ueq,
Uanis(C663) \\sim Ueq, Uanis(C664) \\sim Ueq, Uanis(C665) \\sim Ueq,
Uanis(C666) \\sim Ueq, Uanis(C667) \\sim Ueq, Uanis(C668) \\sim Ueq,
Uanis(C669) \\sim Ueq, Uanis(C670) \\sim Ueq, Uanis(C671) \\sim Ueq,
Uanis(C672) \\sim Ueq, Uanis(C673) \\sim Ueq, Uanis(C101) \\sim Ueq,
Uanis(C102) \\sim Ueq, Uanis(C103) \\sim Ueq, Uanis(C104) \\sim Ueq,
Uanis(C105) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(N222) \\sim Ueq, Uanis(N232)
\\sim Ueq, Uanis(N242) \\sim Ueq, Uanis(N252) \\sim Ueq, Uanis(N262) \\sim Ueq,
Uanis(N612) \\sim Ueq, Uanis(N622) \\sim Ueq, Uanis(N632) \\sim Ueq,
Uanis(N642) \\sim Ueq, Uanis(N652) \\sim Ueq, Uanis(N662) \\sim Ueq,
Uanis(N100) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3)
\\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq,
Uanis(O7) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O223)
\\sim Ueq, Uanis(O233) \\sim Ueq, Uanis(O243) \\sim Ueq, Uanis(O253) \\sim Ueq,
Uanis(O263) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F17)
\\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(F20) \\sim Ueq,
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim
Ueq, Uanis(F5A) \\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F7A) \\sim Ueq,
Uanis(F8A) \\sim Ueq, Uanis(F5B) \\sim Ueq, Uanis(F6B) \\sim Ueq, Uanis(F7B)
\\sim Ueq, Uanis(F8B) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10) \\sim Ueq,
Uanis(F11) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(B1) \\sim Ueq, Uanis(B2A)
\\sim Ueq, Uanis(B2B) \\sim Ueq, Uanis(B3) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(B2A) = Uanis(B2B)
Uanis(F8A) = Uanis(F8B)
4. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: F5A(0.5) F6A(0.5) F7A(0.5) F8A(0.5) B2A(0.5) F5B(0.5) F6B(0.5)
 F7B(0.5) F8B(0.5) B2B(0.5)
5.a Ternary CH refined with riding coordinates:
 N612(H612), N622(H622), N632(H632), N642(H642), N652(H652), N662(H662)
5.b Secondary CH2 refined with riding coordinates:
 C611(H61A,H61B), C613(H61C,H61D), C620(H62A,H62B), C621(H62C,H62D), C1(H1A,
 H1B), C622(H62E,H62F), C623(H62G,H62H), C630(H63A,H63B), C631(H63C,H63D),
 C2(H2A,H2B), C633(H63E,H63F), C640(H64A,H64B), C641(H64C,H64D), C3(H3A,H3B),
 C643(H64E,H64F), C650(H65A,H65B), C651(H65C,H65D), C4(H4A,H4B), C652(H65E,
 H65F), C653(H65G,H65H), C660(H66A,H66B), C661(H66C,H66D), C663(H66E,H66F),
 C670(H67A,H67B), C671(H67C,H67D), C672(H67E,H67F), C673(H67G,H67H)
5.c Me refined with riding coordinates:
 C411(H41A,H41B,H41C), C421(H42A,H42B,H42C), C431(H43A,H43B,H43C), C441(H44A,
 H44B,H44C), C451(H45A,H45B,H45C), C461(H46A,H46B,H46C)
5.d Aromatic/amide H refined with riding coordinates:
 C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38),
 C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C221(H221),
 C231(H231), C241(H241), C251(H251), C261(H261), C615(H615), C616(H616),
 C617(H617), C618(H618), C619(H619), C625(H625), C626(H626), C627(H627),
 C628(H628), C629(H629), C634(H634), C635(H635), C636(H636), C637(H637),
 C638(H638), C645(H645), C646(H646), C647(H647), C648(H648), C649(H649),
 C655(H655), C656(H656), C657(H657), C658(H658), C659(H659), C665(H665),
 C666(H666), C667(H667), C668(H668), C669(H669), C101(H101), C102(H102),
 C103(H103), C104(H104), C105(H105)
;
_smtbx_masks_void_probe_radius   0.2
_smtbx_masks_void_truncation_radius 0.2
_shelx_res_checksum              13330
_shelx_hkl_checksum              73550
_shelx_fab_checksum              52308
_olex2_submission_special_instructions 'No special instructions were received'