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

data_1568211
_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
'C85.333 H100 F8 Fe Hg10 N20 O5.333, 6.333(C2 F3 O2), 1[O2C2F3]'
_chemical_formula_sum            'C100 H100 F30 Fe Hg10 N20 O20'
_chemical_formula_weight         4533.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 109.0010(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8907(4)
_cell_length_b                   40.5278(10)
_cell_length_c                   23.0130(5)
_cell_measurement_reflns_used    9840
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      72.37
_cell_measurement_theta_min      2.30
_cell_volume                     14895.0(6)
_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 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            416111
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.182
_diffrn_reflns_theta_max         67.182
_diffrn_reflns_theta_min         2.305
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    19.591
_exptl_absorpt_correction_T_max  0.7412
_exptl_absorpt_correction_T_min  0.0370
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1431 before and 0.0973 after correction.
The Ratio of minimum to maximum transmission is 0.0499.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.022
_exptl_crystal_description       block
_exptl_crystal_F_000             8384
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.39
_refine_diff_density_max         3.378
_refine_diff_density_min         -1.874
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1710
_refine_ls_number_reflns         26601
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0667P)^2^+228.1016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1439
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24072
_reflns_number_total             26601
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06151a2.cif
_cod_data_source_block           p21_n_final
_cod_depositor_comments
'Adding full bibliography for 1568209--1568211.cif.'
_cod_database_code               1568211
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.049
_shelx_estimated_absorpt_t_min   0.037
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C29-C68 \\sim C29-C105
 with sigma of 0.02
 F18-C68 \\sim F18-C105
 with sigma of 0.02
 F19-C68 \\sim F19-C105
 with sigma of 0.02
 C68-F22 \\sim C105-F22
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C93) = Uanis(C45) = Uanis(C94)
Uanis(C58) = Uanis(C74) = Uanis(C99) = Uanis(N20) = Uanis(C79) = Uanis(C101)
Uanis(C83) = Uanis(N21) = Uanis(C100) = Uanis(C111) = Uanis(C110) = Uanis(C109)
Uanis(C60) = Uanis(N16) = Uanis(C70)
Uanis(C85) = Uanis(N22) = Uanis(C86)
Uanis(C90) = Uanis(N23) = Uanis(C89)
Uanis(C72) = Uanis(N18) = Uanis(C73)
Uanis(O22) = Uanis(O16)
Uanis(O21) = Uanis(O14)
Uanis(C92) = Uanis(C91) = Uanis(C78) = Uanis(C75)
Uanis(C105) = Uanis(C68) = Uanis(C29)
Uanis(C63A) = Uanis(C63) = Uanis(C54) = Uanis(C40)
4. Others
 Fixed Sof: F4(0.5) F8(0.66667) F10(0.5) F11(0.5) F13(0.5) F15(0.5)
 F17(0.66667) F18(0.6) F19(0.6) F20(0.4) F22(0.6) F24(0.5) F26(0.66667)
 F27(0.33333) F28(0.33333) F29(0.33333) F30(0.5) F31(0.5) F32(0.5) F33(0.4)
 F34(0.4) F35(0.5) F38(0.5) O12(0.5) O13(0.66667) O14(0.66667) O16(0.33333)
 O18(0.33333) O20(0.5) O21(0.66667) O22(0.33333) N16(0.5) N18(0.6) N20(0.5)
 N21(0.5) N22(0.5) N23(0.4) C45(0.5) C58(0.5) H58(0.5) C60(0.5) H60A(0.5)
 H60B(0.5) H60C(0.5) C63(0.5) H63A(0.5) H63B(0.5) H63C(0.5) C68(0.6) C70(0.5)
 H70A(0.5) H70B(0.5) H70C(0.5) C72(0.6) H72A(0.6) H72B(0.6) H72C(0.6) C73(0.6)
 H73A(0.6) H73B(0.6) H73C(0.6) C74(0.5) C75(0.66667) C78(0.66667) C79(0.5)
 H79A(0.5) H79B(0.5) H79C(0.5) C83(0.5) H83A(0.5) H83B(0.5) H83C(0.5) C85(0.5)
 H85A(0.5) H85B(0.5) H85C(0.5) C86(0.5) H86A(0.5) H86B(0.5) H86C(0.5) C89(0.4)
 H89A(0.4) H89B(0.4) H89C(0.4) C90(0.4) H90A(0.4) H90B(0.4) H90C(0.4)
 C91(0.33333) C92(0.33333) C93(0.5) H98(0.5) H98A(0.5) C99(0.5) H99(0.5)
 C100(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C101(0.5) H10D(0.5) H10E(0.5)
 H10F(0.5) C105(0.4) H108(0.5) H10G(0.5) C109(0.5) H109(0.5) C110(0.5)
 H110(0.5) C111(0.5) C63A(0.5) H63D(0.5) H63E(0.5) H63F(0.5) F4A(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12), C13(H13), C14(H14), C16(H16), C18(H18), C19(H19),
 C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
  C30(H30), C34(H34), C35(H35), C36(H36), C37(H37), C40(H40), C43(H43),
 C48(H48), C51(H51), C54(H54), C57(H57), C58(H58), C64(H64), C65(H65), C66(H66),
  C76(H76), C84(H84), C87(H87), C88(H88), C96(H96), C98(H98), C98(H98A),
 C99(H99), C106(H106), C107(H107), C108(H108), C108(H10G), C109(H109),
 C110(H110)
5.b Idealised Me refined with everything fixed:
 C100(H10A,H10B,H10C)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C42(H42A,H42B,H42C), C49(H49A,H49B,H49C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,
 H62B,H62C), C63(H63A,H63B,H63C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C),
 C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C77(H77A,H77B,H77C), C79(H79A,H79B,
 H79C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C83(H83A,H83B,H83C), C85(H85A,
 H85B,H85C), C86(H86A,H86B,H86C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C),
 C97(H97A,H97B,H97C), C101(H10D,H10E,H10F), C63A(H63D,H63E,H63F), C69A(H69A,
 H69B,H69C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              13937
_shelx_fab_checksum              66762
_olex2_submission_special_instructions 'No special instructions were received'