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_4121382
_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 N6 O14 S Sc, C H2 Cl2, 2(C F3 O3 S), C4 H10 O2, C4 H9 O'
_chemical_formula_sum            'C77 H77 Cl2 F9 Fe3 N6 O23 S3 Sc'
_chemical_formula_weight         2005.03
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2013-09-26
_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                 102.693(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5972(18)
_cell_length_b                   25.161(3)
_cell_length_c                   23.470(3)
_cell_measurement_reflns_used    9739
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.26
_cell_measurement_theta_min      2.21
_cell_volume                     8409.4(18)
_computing_cell_refinement       'SAINT V8.32B (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 2013.2-0 (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
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            380123
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         35.992
_diffrn_reflns_theta_min         1.619
_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    0.820
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0668 before and 0.0609 after correction.
The Ratio of minimum to maximum transmission is 0.8899.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_description       chunk
_exptl_crystal_F_000             4108
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.40
_refine_diff_density_max         4.306
_refine_diff_density_min         -3.124
_refine_diff_density_rms         0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1162
_refine_ls_number_reflns         37662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.1636
_refine_ls_R_factor_gt           0.1248
_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^)+(0.1066P)^2^+119.8983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3287
_refine_ls_wR_factor_ref         0.3558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26815
_reflns_number_total             37662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja4104974_Sc.cif
_cod_data_source_block           ddl24
_cod_original_cell_volume        8409.4(17)
_cod_database_code               4121382
_cod_database_fobs_code          4121382
_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(S3A)=Sof(F9A)=Sof(O19A)=Sof(C76A)=1-FVAR(1)
 Sof(S3)=Sof(F9)=Sof(O19)=Sof(C76)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C64(H64a,H64b), C65(H65a,H65b), C70(H70a,H70b), C73(H73a,H73b), C74(H74a,
 H74b), C77(H77a,H77b)
3.b Aromatic/amide H refined with riding coordinates:
 O5(H5), C1(H1), C3(H3), C5(H5a), 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), C69(H69)
3.c Idealised Me refined as rotating group:
 C59(H59a,H59b,H59c), C61(H61a,H61b,H61c), C63(H63a,H63b,H63c), C66(H66a,H66b,
 H66c), C68(H68a,H68b,H68c), C71(H71a,H71b,H71c), C72(H72a,H72b,H72c), C75(H75a,
 H75b,H75c)
;