Heterometallic Chiral [Mn13Cu8] Single-Molecule Magnets
Peng, Zhiwei; Li, Shu; Li, Ao; Liao, Jiaming; Wang, Yiman; Li, Xudong; Meng, Wei; Zhang, Jian; Dalton Transactions  (2022) –; doi:10.1039/D1DT04291B

data_7709303
_publ_section_title
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 Heterometallic Chiral [Mn13Cu8] Single-Molecule Magnets
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04291B
_journal_year                    2022
_chemical_absolute_configuration syn
_chemical_formula_moiety
'C49.7 H31.88 Cu8 K4 Mn13 Na6 O94.26, 4.44(H0.5 O0.5), 3.76(H2 O), H O0.81, 0.65(O)'
_chemical_formula_sum            'C49.7 H42.62 Cu8 K4 Mn13 Na6 O101.7'
_chemical_formula_weight         3783.94
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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             2022-01-11
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-01-12 deposited with the CCDC.	2022-01-14 downloaded from the CCDC.
;
_cell_angle_alpha                114.266(3)
_cell_angle_beta                 99.410(3)
_cell_angle_gamma                102.907(3)
_cell_formula_units_Z            1
_cell_length_a                   13.0683(7)
_cell_length_b                   15.7834(10)
_cell_length_c                   16.6333(11)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.82
_cell_measurement_theta_min      2.47
_cell_volume                     2920.1(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.04
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'BRUKER SMART APEXII CCD'
_diffrn_measurement_method       'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_unetI/netI     0.0837
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            59065
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.184
_exptl_absorpt_coefficient_mu    3.065
_exptl_absorpt_correction_T_max  0.4576
_exptl_absorpt_correction_T_min  0.4027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.152
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1853
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.018
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details
;
 Flack x determined using 6085 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1884
_refine_ls_number_reflns         20346
_refine_ls_number_restraints     2679
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0619
_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^)+(0.1041P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1543
_refine_ls_wR_factor_ref         0.1688
_reflns_Friedel_coverage         0.981
_reflns_Friedel_fraction_full    0.980
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                15534
_reflns_number_total             20346
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04291b2.cif
_cod_data_source_block           l-1_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_formula_sum        'C49.70 H42.62 Cu8 K4 Mn13 Na6 O101.70'
_cod_database_code               7709303
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.460
_shelx_estimated_absorpt_t_min   0.405
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H93 of O93, {H97a,H97b} of O97, {H99a,H99b} of O99, {H23a,
  H23b} of O23, {H25a,H25b} of O25, {H47a,H47b} of O47, {H49a,H49} of O49, All
  C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H11e,H11f} of O115, {H11i,H11j} of O119, {H10c,H10d}
  of O105, {H10a,H10b} of O103, {H11c,H11d} of O113, H101 of O101, {H11g,H11h}
  of O117, {H91a,H91b} of O91, {H95a,H95b} of O95, H1 of O1, {H3a,H3b} of O3,
  {H11a,H11b} of O11, {H43a,H43b} of O43
2. Shared sites
{K2, Na4}
3. Uiso/Uaniso restraints and constraints
O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim O9 \\sim O10
\\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O16 \\sim O17 \\sim O18 \\sim O19
\\sim O20 \\sim O21 \\sim O22 \\sim O24 \\sim O26 \\sim O27 \\sim O28 \\sim O29
\\sim O30 \\sim O31 \\sim O32 \\sim O33 \\sim O34 \\sim O35 \\sim O36 \\sim O37
\\sim O38 \\sim O39 \\sim O40 \\sim O41 \\sim O42 \\sim O43 \\sim O44 \\sim O45
\\sim O46 \\sim O48 \\sim O50 \\sim O51 \\sim O52 \\sim O54 \\sim O55 \\sim O56
\\sim O57 \\sim O58 \\sim O59 \\sim O60 \\sim O61 \\sim O62 \\sim O63 \\sim O64
\\sim O65 \\sim O66 \\sim O67 \\sim O68 \\sim O69 \\sim O70 \\sim O71 \\sim O72
\\sim O73 \\sim O74 \\sim O75 \\sim O76 \\sim O77 \\sim O78 \\sim O79 \\sim O80
\\sim O81 \\sim O82 \\sim O83 \\sim O84 \\sim O85 \\sim O86 \\sim O88 \\sim O89
\\sim O90 \\sim O91 \\sim O92 \\sim O94 \\sim O95 \\sim O96 \\sim O98 \\sim
O100 \\sim O102 \\sim O104 \\sim O106 \\sim O107 \\sim O108 \\sim O110 \\sim
O111 \\sim O112 \\sim O114 \\sim O116 \\sim O118 \\sim O120 \\sim O121 \\sim
O122 \\sim O123 \\sim O1 \\sim O15 \\sim O23 \\sim O25 \\sim O47 \\sim O49
\\sim O53 \\sim O87 \\sim O93 \\sim O97 \\sim O99 \\sim O101 \\sim O103 \\sim
O105 \\sim O109 \\sim O113 \\sim O115 \\sim O117 \\sim O119: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
Uanis(O101) \\sim Ueq: with sigma of 0 and sigma for terminal atoms of 0
Uanis(O91) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Na6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C21) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C34) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C6) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C32) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C49) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O52) \\sim Ueq, Uanis(O111) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C25) \\sim Ueq, Uanis(C51) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C37) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C36) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(K2) = Uanis(Na4)
4. Others
 Sof(Cu2)=1-FVAR(1)
 Sof(Cu8)=FVAR(1)
 Fixed Sof: K2(0.5) K6(0.7) K5(0.45) K3(0.35) Na4(0.5) Na6(0.8) Na7(0.7)
 O3(0.6) H3a(0.25) H3b(0.25) O7(0.37) O11(0.5) H11a(0.25) H11b(0.25) O13(0.72)
 O27(0.44) O29(0.6) O45(0.5) O51(0.5) O52(0.5) O54(0.5) O55(0.5) O57(0.39)
 O59(0.35) O61(0.67) O83(0.55) O85(0.57) O89(0.5) O91(0.4) H91a(0.4) H91b(0.4)
 O95(0.5) H95a(0.5) H95b(0.5) O107(0.46) O111(0.5) C3(0.5) H3(0.5) C25(0.6)
 C34(0.5) H36(0.5) H36a(0.5) C49(0.5) C51(0.6) H51a(0.6) H51b(0.6) H51c(0.6)
 O1(0.75) H1(0.75) O15(0.31) O23(0.5) H23a(0.5) H23b(0.5) O25(0.36) H25a(0.36)
 H25b(0.36) O47(0.5) H47a(0.5) H47b(0.5) O49(0.5) H49a(0.5) H49(0.5) O53(0.4)
 O87(0.5) O93(0.47) H93(0.47) O97(0.5) H97a(0.5) H97b(0.5) O99(0.5) H99a(0.5)
 H99b(0.5) O101(0.5) H101(0.5) O103(0.5) H10a(0.5) H10b(0.5) O105(0.38)
 H10c(0.38) H10d(0.38) O109(0.25) O113(0.25) H11c(0.25) H11d(0.25) O115(0.25)
 H11e(0.25) H11f(0.25) O117(0.4) H11g(0.4) H11h(0.4) O119(0.26) H11i(0.26)
 H11j(0.26)
5.a Riding coordinates:
 O3(H3a,H3b), O11(H11a,H11b), O43(H43a,H43b), O91(H91a,H91b), O95(H95a,H95b),
 O1(H1), O23(H23a,H23b), O25(H25a,H25b), O47(H47a,H47b), O49(H49a,H49),
 O93(H93), O97(H97a,H97b), O99(H99a,H99b), O101(H101), O103(H10a,H10b),
 O105(H10c,H10d), O113(H11c,H11d), O115(H11e,H11f), O117(H11g,H11h), O119(H11i,
 H11j)
5.b Ternary CH refined with riding coordinates:
 C4(H4), C6(H6), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C19(H19),
 C20(H20), C21(H21), C22(H22), C23(H23), C28(H28), C29(H29), C30(H30), C33(H33),
  C36(H36), C36(H36a), C37(H37), C38(H38), C41(H41), C44(H44), C45(H45),
 C46(H46), C52(H52)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3)
5.d Idealised Me refined as rotating group:
 C51(H51a,H51b,H51c)
;
_shelx_res_checksum              25082
_shelx_hkl_checksum              82542
_shelx_fab_checksum              4038
_olex2_submission_special_instructions 'No special instructions were received'