An [FeIII30] molecular metal oxide
Dearle, Alice E.; Cutler, Daniel J.; Coletta, Marco; Lee, Edward; Dey, Sourav; Sanz, Sergio; Fraser, Hector W. L.; Nichol, Gary S.; Rajaraman, Gopalan; Schnack, Jürgen; Cronin, Leroy; Brechin, Euan K.; Chemical Communications  (2021) –; doi:10.1039/D1CC06224G

data_7129279
_publ_section_title
;
 An [FeIII30] molecular metal oxide
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06224G
_journal_year                    2021
_chemical_formula_moiety
'C105 H150 Br9 Fe30 N15 O47, 3(Br), 2(C7 H9 N) + solvent'
_chemical_formula_sum            'C119 H169 Br12 Fe30 N17 O47'
_chemical_formula_weight         5224.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-13
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-26 deposited with the CCDC.	2021-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                95.425(2)
_cell_angle_beta                 97.928(2)
_cell_angle_gamma                113.427(2)
_cell_formula_units_Z            2
_cell_length_a                   20.7362(5)
_cell_length_b                   22.7181(4)
_cell_length_c                   25.0130(4)
_cell_measurement_reflns_used    26451
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      75.4910
_cell_measurement_theta_min      3.8320
_cell_volume                     10563.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -112.00 -15.00   1.00   10.00    --  -41.67 -57.00-150.00   97
  2  \w   -116.00 -10.00   1.00   10.00    --  -41.67 -77.00 -30.00  106
  3  \w   -128.00 -35.00   1.00   10.00    --  -41.67-178.00 -30.00   93
  4  \w   -127.00 -34.00   1.00   10.00    --  -41.67 178.00  60.00   93
  5  \w     19.00 114.00   1.00   10.00    --   41.67  38.00  90.00   95
  6  \w     94.00 178.00   1.00   30.00    --  111.00 125.00 150.00   84
  7  \w     66.00 178.00   1.00   30.00    --  111.00  15.00 120.00  112
  8  \w     80.00 178.00   1.00   30.00    --  111.00  77.00-150.00   98
  9  \w     39.00 118.00   1.00   30.00    --  111.00-125.00  30.00   79
 10  \w     39.00 118.00   1.00   30.00    --  111.00-125.00 -90.00   79
 11  \w     41.00 139.00   1.00   30.00    --  111.00 -61.00-180.00   98
 12  \w     30.00 110.00   1.00   30.00    --  111.00 -94.00  90.00   80
 13  \w     87.00 178.00   1.00   30.00    --  111.00  30.00-180.00   91
 14  \w     30.00 110.00   1.00   30.00    --  111.00 -94.00  60.00   80
 15  \w     87.00 178.00   1.00   30.00    --  111.00  45.00 -90.00   91
 16  \w     37.00 142.00   1.00   30.00    --  111.00 -77.00  90.00  105
 17  \w     87.00 178.00   1.00   30.00    --  111.00  30.00 -30.00   91
 18  \w     87.00 178.00   1.00   30.00    --  111.00  30.00-120.00   91
 19  \w     39.00 118.00   1.00   30.00    --  111.00-125.00  60.00   79
 20  \w     66.00 178.00   1.00   30.00    --  111.00  15.00 120.00  112
 21  \w     40.00 136.00   1.00   30.00    --  111.00 -49.00  99.00   96
 22  \w     87.00 178.00   1.00   30.00    --  111.00  45.00 150.00   91
 23  \w     39.00 118.00   1.00   30.00    --  111.00-125.00 -30.00   79
 24  \w     58.00 118.00   1.00   30.00    --  111.00-125.00  90.00   60
 25  \w     49.00  74.00   1.00   30.00    --  111.00-125.00   0.00   25
 26  \w     40.00 135.00   1.00   30.00    --  111.00 -45.00  60.00   95
 27  \w     44.00 131.00   1.00   30.00    --  111.00 -45.00-120.00   87
 28  \w     88.00 140.00   1.00   30.00    --  111.00 -77.00-150.00   52
 29  \w     91.00 118.00   1.00   30.00    --  111.00-125.00-180.00   27
 30  \w    100.00 126.00   1.00   30.00    --  111.00-136.00-128.88   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0305421000
_diffrn_orient_matrix_UB_12      0.0493979000
_diffrn_orient_matrix_UB_13      -0.0381185000
_diffrn_orient_matrix_UB_21      0.0670162000
_diffrn_orient_matrix_UB_22      -0.0143325000
_diffrn_orient_matrix_UB_23      0.0045338000
_diffrn_orient_matrix_UB_31      -0.0371908000
_diffrn_orient_matrix_UB_32      -0.0544787000
_diffrn_orient_matrix_UB_33      -0.0500076000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0982
_diffrn_reflns_av_unetI/netI     0.0918
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            174652
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.143
_diffrn_reflns_theta_min         3.617
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    19.117
_exptl_absorpt_correction_T_max  0.4716
_exptl_absorpt_correction_T_min  0.2130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1183 before and 0.0764 after correction. The Ratio of minimum to maximum transmission is 0.4517. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       block
_exptl_crystal_F_000             5156
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of diethyl ether and acetonitrile  by vapour diffusion'
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.059
_refine_diff_density_max         1.506
_refine_diff_density_min         -1.245
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2012
_refine_ls_number_reflns         43629
_refine_ls_number_restraints     950
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0633
_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^)+(0.1040P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1618
_refine_ls_wR_factor_ref         0.1791
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29952
_reflns_number_total             43629
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06224g2.cif
_cod_data_source_block           eb18084
_cod_database_code               7129279
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H30 N10 O10 Fe Br'
_chemical_oxdiff_usercomment     '@ 120 K  AD443'
_shelx_estimated_absorpt_t_max   0.398
_shelx_estimated_absorpt_t_min   0.141
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups,
  All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C13-C10 = C6-C3 = C20-C17 = C34-C31 = C48-C45 = C62-C59 = C69-C66 = C76-C73 =
 C83-C80 = C90-C87 = C97-C94 = C104-C101 = C27-C24 = C41-C38 = C55-C52 = C111-
 C108 = C118-C115
 1.53 with sigma of 0.02
 C77-C76 = C70-C69 = C63-C62 = C105-C104 = C98-C97 = C49-C48 = C35-C34 = C21-
 C20 = C7-C6 = C14-C13 = C28-C27 = C42-C41 = C56-C55 = C91-C90 = C84-C83 = C112-
 C111 = C119-C118
 1.45 with sigma of 0.02
 C7A-C6
 1.45 with sigma of 0.02
 C14A-C13
 1.45 with sigma of 0.02
 O3-H3 = O7-H7 = O4-H4 = O35-H35 = O45-H45 = O46-H46 = O16-H16 = O27-H27 = O5-
 H5 = O10-H10 = O31-H31 = O21-H21 = O6-H6 = O23-H23 = O38-H38 = O39-H39
 0.84 with sigma of 0.02
 C56-C52 = C42-C38 = C28-C24 = C7-C3 = C14-C10 = C91-C87 = C84-C80 = C98-C94 =
 C105-C101 = C63-C59 = C49-C45 = C31-C35 = C21-C17 = C115-C119 = C112-C108 =
 C66-C70 = C77-C73
 2.48 with sigma of 0.04
 C14A-C10 = C7A-C3
 2.48 with sigma of 0.04
3. Rigid body (RIGU) restrains
 N4, C22, C23, C24, C25, C26, C27, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N6, C36, C37, C38, C39, C40, C41, C42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N8, C50, C51, C52, C53, C54, C55, C56
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N11, C71, C72, C73, C74, C75, C76, C77
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N10, C64, C65, C66, C67, C68, C69, C70
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N9, C57, C58, C59, C60, C61, C62, C63
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C1, C2, C3, C4, C5, C6, C7, C7A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2, C8, C9, C10, C11, C12, C13, C14, C14A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N13, C85, C86, C87, C88, C89, C90, C91
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N12, C78, C79, C80, C81, C82, C83, C84
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N7, C43, C44, C45, C46, C47, C48, C49
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N5, C29, C30, C31, C32, C33, C34, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, C15, C16, C17, C18, C19, C20, C21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N15, C99, C100, C101, C102, C103, C104, C105
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N14, C92, C93, C94, C95, C96, C97, C98
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N16, C106, C110, C107, C109, C108, C111, C112
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N17, C113, C117, C114, C116, C115, C118, C119
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H6BC)=Sof(H6BD)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(H13C)=
 Sof(H13D)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(1)
 Sof(H6AA)=Sof(H6AB)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(H13A)=Sof(H13B)=
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(1)
5.a Everything fixed:
 H3, H4, H5, H6, H7, H10, H16, H21, H23, H27, H31, H35, H38, H39, H45, H46, C7A
5.b Secondary CH2 refined with riding coordinates:
 C6(H6AA,H6AB), C6(H6BC,H6BD), C13(H13A,H13B), C13(H13C,H13D), C20(H20A,H20B),
 C27(H27A,H27B), C34(H34A,H34B), C48(H48A,H48B), C55(H55A,H55B), C62(H62A,H62B),
  C69(H69A,H69B), C76(H76A,H76B), C83(H83A,H83B), C90(H90A,H90B), C97(H97A,
 H97B), C104(H10A,H10B), C111(H11A,H11B), C118(H11F,H11G)
5.c Me refined with riding coordinates:
 C7(H7A,H7B,H7C), C7A(H7AA,H7AB,H7AC), C14(H14A,H14B,H14C), C14A(H14D,H14E,
 H14F), C21(H21A,H21B,H21C), C28(H28A,H28B,H28C), C35(H35A,H35B,H35C), C42(H42A,
 H42B,H42C), C49(H49A,H49B,H49C), C56(H56A,H56B,H56C), C63(H63A,H63B,H63C),
 C70(H70A,H70B,H70C), C77(H77A,H77B,H77C), C84(H84A,H84B,H84C), C91(H91A,H91B,
 H91C), C98(H98A,H98B,H98C), C105(H10C,H10D,H10E), C112(H11C,H11D,H11E),
 C119(H11H,H11I,H11J)
5.d Aromatic/amide H refined with riding coordinates:
 C85(H85), C86(H86), C88(H88), C89(H89), C1(H1), C2(H2), C4(H4A), C5(H5A),
 C8(H8), C9(H9), C11(H11), C12(H12), C15(H15), C16(H16A), C18(H18), C19(H19),
 C22(H22), C23(H23A), C25(H25), C26(H26), C29(H29), C30(H30), C32(H32),
 C33(H33), C36(H36), C37(H37), C39(H39A), C40(H40), C41(H41), C43(H43),
 C44(H44), C46(H46A), C47(H47), C50(H50), C51(H51), C53(H53), C54(H54),
 C57(H57), C58(H58), C60(H60), C61(H61), C64(H64), C65(H65), C67(H67), C68(H68),
  C71(H71), C72(H72), C74(H74), C75(H75), C78(H78), C79(H79), C81(H81),
 C82(H82), C92(H92), C93(H93), C95(H95), C96(H96), C99(H99), C100(H100),
 C102(H102), C103(H103), N16(H16B), C106(H106), C107(H107), C109(H109),
 C110(H110), C113(H113), C114(H114), C116(H116), C117(H117)
5.e Fitted hexagon refined as free rotating group:
 N13(C85,C86,C87,C88,C89), N16(C106,C107,C108,C109,C110)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              44761
_shelx_fab_checksum              9505
_olex2_date_sample_data_collection 2018-09-14
_olex2_date_sample_submission    2018-09-10
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id AD443
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 2.034
_oxdiff_exptl_absorpt_empirical_full_min 0.610