Constructing an unprecedented {Mn<sup>II</sup><sub>38</sub>} matryoshka doll with a [Mn<sub>18</sub>(CO<sub>3</sub>)<sub>9</sub>] inorganic core and magnetocaloric effect.
Wu, Tai-Xue; Tao, Ye; He, Qiu-Ju; Li, Hai-Ye; Bian, He-Dong; Huang, Fu-Ping; Chemical communications (Cambridge, England) 57 (2021) 2732–2735; doi:10.1039/d0cc07884k

data_7127960
_publ_section_title
;
 Constructing an unprecedented {Mn<sup>II</sup><sub>38</sub>} matryoshka
 doll with a [Mn<sub>18</sub>(CO<sub>3</sub>)<sub>9</sub>] inorganic core
 and magnetocaloric effect.
;
_journal_issue                   22
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2732
_journal_page_last               2735
_journal_paper_doi               10.1039/d0cc07884k
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety
'C297 H228 Cl24 Mn38 N144 O33, 2(Cl4 Mn1), 6(C2 H8 N)'
_chemical_formula_sum            'C309 H276 Cl32 Mn40 N150 O33'
_chemical_formula_weight         9950.78
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2020-09-17 deposited with the CCDC.	2021-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   25.0072(12)
_cell_length_b                   25.0072(12)
_cell_length_c                   55.114(2)
_cell_measurement_reflns_used    6595
_cell_measurement_temperature    298.3(10)
_cell_measurement_theta_max      65.2230
_cell_measurement_theta_min      3.5170
_cell_volume                     29849(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.3(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -27.00  18.00   0.50   10.00    --  -47.62  19.00  30.00   90
  2  \w    -42.00 -17.00   0.50   75.00    --  -88.50  37.00 150.00   50
  3  \w    -42.00 -16.00   0.50   75.00    --  -88.50  37.00   0.00   52
  4  \w    -59.00 -23.00   0.50   75.00    --  -88.50  57.00 -60.00   72
  5  \w    -64.00 -16.00   0.50   75.00    --  -88.50  57.00-150.00   96
  6  \w    -90.00 -16.00   0.50   75.00    --  -88.50 131.00 -89.00  148
  7  \w   -160.00 -79.00   0.50   75.00    --  -88.50 -86.00  25.00  162
  8  \w   -103.00 -77.00   0.50   10.00    --  -47.62-125.00 -60.00   52
  9  \w   -117.00 -74.00   0.50   10.00    --  -47.62-125.00 -90.00   86
 10  \w     36.00 107.00   0.50   75.00    --  108.56-106.00  20.00  142
 11  \w     86.00 115.00   0.50   75.00    --  108.56-138.00  23.00   58
 12  \w     37.00  65.00   0.50   75.00    --  108.56 -57.00 120.00   56
 13  \w    101.00 168.00   0.50   75.00    --  108.56  19.00 120.00  134
 14  \w     43.00  76.00   0.50   75.00    --  108.56-138.00  23.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0456664000
_diffrn_orient_matrix_UB_12      -0.0522926000
_diffrn_orient_matrix_UB_13      -0.0167634000
_diffrn_orient_matrix_UB_21      0.0196207000
_diffrn_orient_matrix_UB_22      -0.0439666000
_diffrn_orient_matrix_UB_23      0.0111973000
_diffrn_orient_matrix_UB_31      -0.0509364000
_diffrn_orient_matrix_UB_32      -0.0197630000
_diffrn_orient_matrix_UB_33      0.0193641000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1231
_diffrn_reflns_av_unetI/netI     0.0867
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            42960
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.077
_diffrn_reflns_theta_max         67.077
_diffrn_reflns_theta_min         3.535
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.540
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83397
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       block
_exptl_crystal_F_000             14964
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     873
_refine_ls_number_reflns         11723
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1854
_refine_ls_R_factor_gt           0.1009
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2738
_refine_ls_wR_factor_ref         0.3433
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5337
_reflns_number_total             11723
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07884k2.cif
_cod_data_source_block           20200713-hfp-wtx-0706-7-mn
_cod_depositor_comments          'Adding full bibliography for 7127960.cif.'
_cod_original_cell_volume        29849(3)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7127960
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C18 H18 O18 N18 Mn18 Cl18 '
_shelx_estimated_absorpt_t_max   0.188
_shelx_estimated_absorpt_t_min   0.008
_reflns_odcompleteness_completeness 99.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C51-O6
 1.25 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O4) = Uanis(O4A)
Uanis(O3) = Uanis(O3A)
Uanis(O2) = Uanis(O2A)
Uanis(O1) = Uanis(O1A)
4. Others
 Sof(O2A)=Sof(O3A)=Sof(O1A)=Sof(O4A)=1-FVAR(1)
 Sof(O1)=Sof(O4)=Sof(O2)=Sof(O3)=FVAR(1)
 Fixed Sof: O6(0.5)
5.a Secondary CH2 refined with riding coordinates:
 N25(H25A,H25B)
5.b Aromatic/amide H refined with riding coordinates:
 N19(H19), N21(H21), C1(H1), C2(H2), C5(H5), C12(H12), C15(H15), C16(H16),
 C17(H17), C18(H18), C21(H21A), C28(H28), C31(H31), C32(H32), C33(H33),
 C34(H34), C37(H37), C44(H44), C47(H47), C48(H48)
5.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C14(H14A,H14B,H14C), C20(H20A,H20B,H20C), C30(H30A,H30B,
 H30C), C36(H36A,H36B,H36C), C46(H46A,H46B,H46C), C52(H52A,H52B,H52C), C53(H53A,
 H53B,H53C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              10866
_shelx_hkl_checksum              13972
_shelx_fab_checksum              31180
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.274
_oxdiff_exptl_absorpt_empirical_full_min 0.791