Heterometallic Triiron-Oxo/Hydroxo Clusters: Effect of Redox-Inactive Metals
David E. Herbert; Davide Lionetti; Jonathan Rittle; Theodor Agapie; Journal of the American Chemical Society 135 (2013) 19075–19078; doi:10.1021/ja4104974

data_4121385
_publ_contact_author_address
;
Beckman Institute
Caltech 139-74
Pasadena CA 91125
USA
;
_publ_contact_author_email       xray@caltech.edu
_publ_contact_author_name        'Xray Staff'
_publ_section_title
;
 Heterometallic Triiron-Oxo/Hydroxo Clusters: Effect of Redox-Inactive
 Metals
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19075
_journal_page_last               19078
_journal_paper_doi               10.1021/ja4104974
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety
'C66 H56 Ca F3 Fe3 N6 O14 S, C F3 O3 S, C4 H10 O2, 1.56(C4 H10 O)'
_chemical_formula_sum            'C77.25 H81.63 Ca F6 Fe3 N6 O20.56 S2'
_chemical_formula_weight         1808.93
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2013-10-11
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
 SHELXL-2013,
 and manual edit
;
_cell_angle_alpha                90
_cell_angle_beta                 93.023(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8543(18)
_cell_length_b                   26.583(4)
_cell_length_c                   25.731(4)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    100
_cell_measurement_theta_max      22.66
_cell_measurement_theta_min      2.20
_cell_volume                     8097(2)
_computing_cell_refinement       'SAINT V8.32B (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 2013.6-2 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT V8.32B (Bruker-AXS, 2007)'
_computing_molecular_graphics    'DIAMOND 3 (Crystal Impact, 1999)'
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
 and SHELXTL (Bruker-AXS, 2007)
;
_computing_structure_refinement  'SHELXL-2013/2 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT (Sheldrick, 2012)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1223
_diffrn_reflns_av_unetI/netI     0.1168
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            100724
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.310
_diffrn_reflns_theta_min         1.532
_diffrn_source_current           30
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7084
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0954 before and 0.0841 after correction.
The Ratio of minimum to maximum transmission is 0.7084.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       prism
_exptl_crystal_F_000             3743
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.178
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1060
_refine_ls_number_reflns         18166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1744
_refine_ls_R_factor_gt           0.0986
_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^)+(0.1060P)^2^+60.7736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2377
_refine_ls_wR_factor_ref         0.2798
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10325
_reflns_number_total             18166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja4104974_redCa.cif
_cod_data_source_block           a13138q2
_cod_database_code               4121385
_cod_database_fobs_code          4121385
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. others
 Sof(C66A)=Sof(H66D)=Sof(H66E)=Sof(H66F)=1-FVAR(1)
 Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=FVAR(1)
 Sof(O22)=Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(H80C)=Sof(C81)=Sof(H81A)=Sof(H81B)=
 Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=Sof(C83)=Sof(H83A)=Sof(H83B)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C64(H64A,H64B), C65(H65A,H65B), C69(H69A,H69B), C70(H70A,H70B), C77(H77A,
 H77B), C78(H78A,H78B), C81(H81A,H81B), C83(H83A,H83B)
3.b Aromatic/amide H refined with riding coordinates:
 O5(H5), C2(H2), C4(H4), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C15(H15),
 C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25),
  C26(H26), C27(H27), C28(H28), C32(H32), C33(H33), C34(H34), C35(H35),
 C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45),
  C49(H49), C50(H50), C51(H51), C52(H52), C54(H54), C55(H55), C56(H56), C57(H57)
3.c Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C66(H66A,H66B,
 H66C), C66A(H66D,H66E,H66F), C68(H68A,H68B,H68C), C71(H71A,H71B,H71C),
 C76(H76A,H76B,H76C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C82(H82A,H82B,
 H82C)
;