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_4121381
_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 F3 Fe3 La N6 O14 S, 0.39(C H2 Cl2), 1.61(C4 H10 O),
 2(C F3 O3 S), C4 H10 O2
;
_chemical_formula_sum            'C79.87 H82.97 Cl0.76 F9 Fe3 La N6 O22.62 S3'
_chemical_formula_weight         2089.28
_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             2013-10-10
_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                 102.574(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.949(5)
_cell_length_b                   25.335(8)
_cell_length_c                   23.827(8)
_cell_measurement_reflns_used    9191
_cell_measurement_temperature    100
_cell_measurement_theta_max      34.18
_cell_measurement_theta_min      2.41
_cell_volume                     8808(5)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'APEX2 2013.2-0 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.954
_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  0.0617
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            257785
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         34.843
_diffrn_reflns_theta_min         1.611
_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    1.147
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0746 before and 0.0562 after correction.
The Ratio of minimum to maximum transmission is 0.7564.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_description       plate
_exptl_crystal_F_000             4248
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.955
_refine_diff_density_min         -1.446
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1148
_refine_ls_number_reflns         36543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0786P)^2^+21.7783P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1458
_refine_ls_wR_factor_ref         0.1726
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25898
_reflns_number_total             36543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja4104974_La.cif
_cod_data_source_block           mkt
_cod_database_code               4121381
_cod_database_fobs_code          4121381
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.576
_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(Cl1)=Sof(Cl2)=Sof(C87)=Sof(H87A)=Sof(H87B)=1-FVAR(1)
 Sof(O25)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=Sof(C83)=Sof(H83A)=Sof(H83B)=
 Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(H85C)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 O12(H12)
3.b Secondary CH2 refined with riding coordinates:
 C64(H64A,H64B), C83(H83A,H83B), C84(H84A,H84B), C87(H87A,H87B), C70(H70A,
 H70B), C72(H72A,H72B), C74(H74A,H74B), C76(H76A,H76B)
3.c Aromatic/amide H refined with riding coordinates:
 O5(H5), C2(H2), C4(H4), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12A),
 C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24),
  C29(H29), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36),
 C37(H37), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46),
  C47(H47), C49(H49), C50(H50), C51(H51), C52(H52), C54(H54), C55(H55),
 C56(H56), C57(H57), C63(H63)
3.d Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C65(H65A,H65B,
 H65C), C82(H82A,H82B,H82C), C85(H85A,H85B,H85C), C69(H69A,H69B,H69C), C71(H71A,
 H71B,H71C), C73(H73A,H73B,H73C), C77(H77A,H77B,H77C)
;