A decacationic ferrocene-based metallostar.
Rupf, Susanne Margot; Moshtaha, Amina Leoni; Malischewski, Moritz; Chemical science 14 (2023) 1132–1137; doi:10.1039/d2sc06151a

data_1568210
_publ_section_title
;
 A decacationic ferrocene-based metallostar.
;
_journal_issue                   5
_journal_name_full               'Chemical science'
_journal_page_first              1132
_journal_page_last               1137
_journal_paper_doi               10.1039/d2sc06151a
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety
'C50 H78 Fe Hg10 S10, 8(F6 Sb), 20(C2 H3 N), 1[Sb2F16N4C8H12]'
_chemical_formula_sum            'C98 H150 F60 Fe Hg10 N24 S10 Sb10'
_chemical_formula_weight         6404.26
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-22
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2022-10-19 deposited with the CCDC.	2022-12-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.377(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7149(8)
_cell_length_b                   36.9102(16)
_cell_length_c                   32.7166(14)
_cell_measurement_reflns_used    9192
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.11
_cell_measurement_theta_min      2.17
_cell_volume                     22533.8(17)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0376
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            325039
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.164
_diffrn_reflns_theta_max         25.164
_diffrn_reflns_theta_min         1.983
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.197
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0999 before and 0.0466 after correction.
The Ratio of minimum to maximum transmission is 0.5651.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.888
_exptl_crystal_description       block
_exptl_crystal_F_000             11768
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN at -30\%C'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.33
_refine_diff_density_max         2.136
_refine_diff_density_min         -1.874
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         20131
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+442.4666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1095
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18394
_reflns_number_total             20131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06151a2.cif
_cod_data_source_block           c2_c_final
_cod_depositor_comments
'Adding full bibliography for 1568209--1568211.cif.'
_cod_database_code               1568210
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.173
_shelx_estimated_absorpt_t_min   0.105
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Sb10, Sb5}
{Sb3, Sb1}
{F31, F10}
3. Uiso/Uaniso restraints and constraints
Uanis(F30) = Uanis(F15) = Uanis(F33) = Uanis(F13) = Uanis(F11) = Uanis(F32) =
Uanis(F12) = Uanis(F34) = Uanis(F14) = Uanis(F35) = Uanis(F31) = Uanis(F10)
Uanis(C51) = Uanis(C52) = Uanis(C54) = Uanis(C53) = Uanis(C50)
Uanis(C23) = Uanis(C22)
Uanis(F73) = Uanis(F70)
Uanis(F61) = Uanis(F62) = Uanis(F64) = Uanis(F63) = Uanis(F60) = Uanis(F91) =
Uanis(F90) = Uanis(F95) = Uanis(F94) = Uanis(F93) = Uanis(F92)
Uanis(F85) = Uanis(F82) = Uanis(F80) = Uanis(F81) = Uanis(F83) = Uanis(F40) =
Uanis(F42) = Uanis(F41) = Uanis(F84) = Uanis(F43)
Uanis(F105) = Uanis(F104) = Uanis(F103) = Uanis(F102) = Uanis(F100) =
Uanis(F101)
Uanis(Sb10) = Uanis(Sb5)
Uanis(C21) = Uanis(C22) = Uanis(C23)
Uanis(Sb3) = Uanis(Sb1)
Uanis(F31) = Uanis(F10)
4. Others
 Fixed Sof: Sb1(0.5) F10(0.5) H55A(0.5) H55B(0.5) H55C(0.5) H55D(0.5)
 H50C(0.5) H50D(0.5) H50A(0.5) H50B(0.5) F21(0.5) F23(0.5) H24A(0.5) H24B(0.5)
 C302(0.5) H30C(0.5) H30D(0.5) H30E(0.5) C22(0.5) H22A(0.5) H22B(0.5) C53(0.5)
 H53A(0.5) H53B(0.5) Sb2(0.5) F25(0.5) C51(0.5) H51A(0.5) H51B(0.5) Sb3(0.5)
 F30(0.5) F14(0.5) F34(0.5) F15(0.5) F33(0.5) F13(0.5) F11(0.5) F31(0.5)
 F74(0.5) F40(0.5) Sb4(0.5) Sb5(0.25) Sb6(0.25) F62(0.25) F64(0.25) F32(0.5)
 C301(0.5) H30F(0.5) H30G(0.5) H30H(0.5) F35(0.5) F12(0.5) C54(0.5) H54A(0.5)
 H54B(0.5) C52(0.5) H52A(0.5) H52B(0.5) C23(0.5) H23A(0.5) H23B(0.5) F90(0.25)
 F61(0.25) F95(0.25) F94(0.25) F63(0.25) F22(0.5) F24(0.5) F70(0.5) F71(0.5)
 F72(0.5) F75(0.5) Sb7(0.5) Sb8(0.5) F85(0.5) F80(0.5) F81(0.5) F82(0.5)
 F42(0.5) F41(0.5) F73(0.5) F103(0.5) F101(0.5) F105(0.5) F60(0.25) F93(0.25)
 F91(0.5) F92(0.25) Sb9(0.25) F43(0.5) F102(0.5) F104(0.5) F100(0.5) Sb10(0.25)
 H21C(0.5) H21D(0.5) H21A(0.5) H21B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C55(H55A,H55B), C55(H55C,H55D), C50(H50C,H50D), C50(H50A,
 H50B), C30(H30A,H30B), C24(H24A,H24B), C20(H20A,H20B), C13(H13A,H13B),
 C12(H12A,H12B), C11(H11A,H11B), C42(H42A,H42B), C41(H41A,H41B), C40(H40A,H40B),
  C33(H33A,H33B), C32(H32A,H32B), C43(H43A,H43B), C31(H31A,H31B), C22(H22A,
 H22B), C53(H53A,H53B), C51(H51A,H51B), C54(H54A,H54B), C52(H52A,H52B),
 C23(H23A,H23B), C21(H21C,H21D), C21(H21A,H21B)
5.b Idealised Me refined as rotating group:
 C101(H10C,H10D,H10E), C601(H60A,H60B,H60C), C501(H50E,H50F,H50G), C302(H30C,
 H30D,H30E), C401(H40C,H40D,H40E), C701(H70A,H70B,H70C), C801(H80A,H80B,H80C),
 C201(H20C,H20D,H20E), C900(H90A,H90B,H90C), C111(H11C,H11D,H11E), C301(H30F,
 H30G,H30H)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              96536
_shelx_fab_checksum              12033
_olex2_submission_special_instructions 'No special instructions were received'