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

data_1568209
_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
'C30 H30 Fe Hg10 N10, 8(F6 Sb), F6 Mo0.5 Sb0.5, 4(F1.5 Sb0.375), 4(F1.5 Mo0.125), 2(O2 S), 10(F)'
_chemical_formula_sum            'C30 H30 F76 Fe Hg10 Mo N10 O4 S2 Sb10'
_chemical_formula_weight         5477.95
_chemical_properties_physical    Moisture-sensitive
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-19
_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                78.893(3)
_cell_angle_beta                 83.202(2)
_cell_angle_gamma                80.190(3)
_cell_formula_units_Z            1
_cell_length_a                   11.5091(7)
_cell_length_b                   16.0047(12)
_cell_length_c                   16.9690(11)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.46
_cell_volume                     3010.4(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_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  0.0291
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            66569
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.297
_diffrn_reflns_theta_min         2.090
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.292
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0945 before and 0.0433 after correction.
The Ratio of minimum to maximum transmission is 0.5475.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    3.022
_exptl_crystal_description       block
_exptl_crystal_F_000             2406
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: HF and SO2 at -80\%C'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.691
_refine_diff_density_min         -2.278
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         14855
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+54.1105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0697
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13680
_reflns_number_total             14855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06151a2.cif
_cod_data_source_block           p-1
_cod_depositor_comments
'Adding full bibliography for 1568209--1568211.cif.'
_cod_database_code               1568209
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.208
_shelx_estimated_absorpt_t_min   0.109
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Sb61, Mo5}
{Sb5, Mo6}
{F60, F5}
{F55, F6}
{F16, F53}
{F7, F51}
{F8, F65}
{F9, F63}
{F17, F64}
{F18, F50}
{F66, F62}
{F54, F26}
{F94, F52}
{F19, F4}
{Sb7, Mo7}
3. Uiso/Uaniso restraints and constraints
: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(Sb5) = Uanis(Mo6)
Uanis(Sb61) = Uanis(Mo5)
Uiso(F60) = Uiso(F5)
Uiso(F8) = Uiso(F65)
Uiso(F7) = Uiso(F51)
Uiso(F55) = Uiso(F6)
Uiso(F16) = Uiso(F53)
Uiso(F9) = Uiso(F63)
Uiso(F17) = Uiso(F64)
Uiso(F18) = Uiso(F50)
Uiso(F66) = Uiso(F62)
Uiso(F54) = Uiso(F26)
Uiso(F94) = Uiso(F52)
Uiso(F19) = Uiso(F4)
Uanis(Sb7) = Uanis(Mo7)
4. Others
 Fixed Sof: Sb7(0.25) Sb61(0.375) Sb5(0.375) Mo5(0.125) Mo6(0.125) Mo7(0.25)
 F7(0.25) F50(0.25) F52(0.25) F53(0.25) F54(0.25) F55(0.25) F4(0.25) F60(0.25)
 F63(0.25) F64(0.25) F65(0.25) F66(0.25) F6(0.25) F16(0.25) F18(0.25) F26(0.25)
 F51(0.25) F94(0.25) F5(0.25) F8(0.25) F9(0.25) F17(0.25) F19(0.25) F62(0.25)
5.a Idealised Me refined with everything fixed:
 C41(H41A,H41B,H41C)
5.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C21(H21A,H21B,H21C), C31(H31A,H31B,H31C), C51(H51A,H51B,
 H51C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              34282
_shelx_fab_checksum              40450
_olex2_submission_special_instructions 'No special instructions were received'