Molecular multifunctionality preservation upon surface deposition for a chiral Single-Molecule Magnet
Mitcov, Dmitri; Pedersen, Anders Hjordt; Ceccato, Marcel; Gelardi, Rikke Munch; Hassenkam, Tue; Konstantatos, Andreas; Reinholdt, Anders; Sørensen, Mikkel A.; Thulstrup, Peter Waaben Waaben; Vinum, Morten Gotthold; Wilhelm, Fabrice; Rogalev, Andrei; Wernsdorfer, Wolfgang; Brechin, Euan K.; Piligkos, Stergios; Chemical Science  (2019) –; doi:10.1039/C8SC04917C

data_1550524
_publ_section_title
;
 Molecular multifunctionality preservation upon surface deposition for a
 chiral Single-Molecule Magnet
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04917C
_journal_year                    2019
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C78 H102 Mn9 N6 O28 S6, Cl'
_chemical_formula_sum            'C78 H102 Cl Mn9 N6 O28 S6'
_chemical_formula_weight         2293.92
_chemical_name_systematic        'Mn9-lipoate Delta-Delta enantiomer'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-04-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2018-04-26 deposited with the CCDC.
2019-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4007(6)
_cell_length_b                   25.1409(11)
_cell_length_c                   26.8999(12)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    122
_cell_measurement_theta_max      26.182
_cell_measurement_theta_min      2.347
_cell_volume                     9062.7(7)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            374822
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.221
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.458
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1044 before and 0.0767 after correction. The Ratio of minimum to maximum transmission is 0.9029. 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    1.681
_exptl_crystal_description       prism
_exptl_crystal_F_000             4696
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'ether diffusion into methanol solution containing the reaction mixture'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.847
_refine_diff_density_min         -1.614
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details
;
 Flack x determined using 6329 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.000(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1129
_refine_ls_number_reflns         15955
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0623P)^2^+34.2771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1249
_reflns_Friedel_coverage         0.833
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                14730
_reflns_number_total             15955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04917c2.cif
_cod_data_source_block           mo_d8v3226_0m
_cod_database_code               1550524
_shelxl_version_number           2013-3
_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, All O(H) groups
2. Restrained distances
 O17-H17
 0.85 with sigma of 0.01
 O22-H22
 0.85 with sigma of 0.01
 O28-H28
 0.85 with sigma of 0.01
 C1AA-C2AA
 1.4 with sigma of 0.02
 C3AA-C4AA
 1.4 with sigma of 0.02
 C4-C1AA
 1.4 with sigma of 0.02
 H4AB-H1AA
 2.1 with sigma of 0.02
 C110-H17
 1.888108 with sigma of 0.02
 Mn8-H17
 2.732422 with sigma of 0.02
 C34-H22
 1.887233 with sigma of 0.02
 Mn4-H22
 2.815721 with sigma of 0.02
 C63-H28
 1.882522 with sigma of 0.02
 Mn9-H28
 2.760737 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(S1) = Uanis(S4) = Uanis(S1AA) = Uanis(S0AA)
Uanis(C13) = Uanis(C18) = Uanis(C5AA)
Uanis(S5) = Uanis(S2AA) = Uanis(S1AA) = Uanis(S0AA)
Uanis(C6) = Uanis(C5)
Uanis(C3AA) = Uanis(C2)
Uanis(C119) = Uanis(C16) = Uanis(C3AA) = Uanis(C4AA) = Uanis(C4) = Uanis(C1AA)
= Uanis(C2AA)
4. Others
 Fixed Sof: S0AA(0.5) S1AA(0.5) C1AA(0.5) C3AA(0.5) C2AA(0.5) H2AA(0.5)
 H2AB(0.5) S2AA(0.5) C5(0.5) H5A(0.5) H5B(0.5) S5(0.5) C6(0.5) C2(0.5)
5.a Ternary CH refined with riding coordinates:
 C8(H8), C13(H13), C4(H4)
5.b Secondary CH2 refined with riding coordinates:
 C94(H94A,H94B), C119(H11D,H11E), C131(H13A,H13B), C7(H7A,H7B), C0AA(H0AA,
 H0AB), C10(H10A,H10B), C11(H11F,H11G), C12(H12A,H12B), C14(H14A,H14B),
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C5AA(H5AA,
 H5AB), C4AA(H4AA,H4AB), C1AA(H1AA,H1AB), C3AA(H3AA,H3AB), C2AA(H2AA,H2AB),
 C5(H5A,H5B)
5.c Aromatic/amide H refined with riding coordinates:
 C36(H36), C39(H39), C42(H42), C49(H49), C56(H56), C60(H60), C65(H65),
 C66(H66), C67(H67), C69(H69), C75(H75), C76(H76), C77(H77), C78(H78), C81(H81),
  C83(H83), C86(H86), C87(H87), C88(H88), C100(H100), C101(H101), C102(H102),
 C106(H106), C107(H107)
5.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C55(H55A,H55B,H55C), C57(H57A,H57B,H57C), C61(H61A,H61B,
 H61C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C68(H68A,H68B,H68C), C72(H72A,
 H72B,H72C), C96(H96A,H96B,H96C), C98(H98A,H98B,H98C), C110(H11A,H11B,H11C),
 C9(H9A,H9B,H9C)
;
_shelx_res_checksum              81609
_olex2_submission_special_instructions 'No special instructions were received'