Solvent Dependence of Crystal Structure and Dielectric Relaxation in Ferromagnetic [MnCr(oxalate)3]− Salt
WU, Jiabing; Huang, Rui-Kang; Takahashi, Kiyonori; Nakamura, Takayoshi; Dalton Transactions  (2022) –; doi:10.1039/D2DT01615J

data_7710589
_publ_section_title
;
 Solvent Dependence of Crystal Structure and Dielectric Relaxation in
 Ferromagnetic [MnCr(oxalate)3]&#x2212; Salt
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01615J
_journal_year                    2022
_chemical_formula_moiety         '0.5(C12 Cr2 Mn2 O24), C12 H24 O6, C5 H12 N O2'
_chemical_formula_sum            'C23 H36 Cr Mn N O20'
_chemical_formula_weight         753.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-05-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-18 deposited with the CCDC.	2022-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.318(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9417(6)
_cell_length_b                   17.0164(8)
_cell_length_c                   10.4599(9)
_cell_measurement_reflns_used    3906
_cell_measurement_temperature    93.2(3)
_cell_measurement_theta_max      30.7870
_cell_measurement_theta_min      2.3710
_cell_volume                     1574.79(19)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93.15
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.853
_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     -7.00  73.00   0.50   10.35    --    5.13  41.00 -18.00  160
  2  \w    -65.00 -17.00   0.50   10.35    --    5.13 -41.00-171.00   96
  3  \w    -10.00  26.00   0.50   10.35    --   -4.97 -99.00-120.00   72
  4  \w    -15.00  22.00   0.50   10.35    --   -4.97 -99.00-180.00   74
  5  \w    -66.00   6.00   0.50   10.35    --   -4.97 -37.00  90.00  144
  6  \w    -10.00  29.00   0.50   10.35    --    5.13 -99.00 150.00   78
  7  \w    -18.00  30.00   0.50   10.35    --    5.13 -99.00  60.00   96
  8  \w    -18.00  39.00   0.50   10.35    --    5.13 -99.00-150.00  114
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.853
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10250
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.751
_diffrn_reflns_theta_min         2.394
_exptl_absorpt_coefficient_mu    0.833
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.503
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.52(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         3915
_refine_ls_number_restraints     200
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0779
_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^)+(0.1154P)^2^+4.0225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.2044
_reflns_Friedel_coverage         0.941
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.854
_reflns_number_gt                2998
_reflns_number_total             3915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01615j2.cif
_cod_data_source_block           valeric_18c6
_cod_database_code               7710589
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.48(7)
 0.52(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 C16-C15 = C18-C17 = C19-C20 = C10-C9 = C11-C12 = C13-C14
 1.48 with sigma of 0.02
 C10-C11 = C14-C15 = C20-C9 = C16-C17 = C12-C13 = C18-C19
 2.6 with sigma of 0.06
 C19-O3 = O5-C14 = O3-C10 = C13-O6 = C11-O5 = O8-C20 = O6-C16 = C15-O7 = C9-O4
 = O4-C12 = O7-C18 = C17-O8
 2.5 with sigma of 0.06
 O3-C9 = O3-C20 = O8-C19 = O8-C18 = O7-C17 = O7-C16 = O6-C15 = O6-C14 = O5-C13
 = O5-C12 = O4-C10 = O4-C11
 1.4 with sigma of 0.02
 C2-C1 = C3-C2 = C4-C3 = C5-C4
 1.5 with sigma of 0.02
 O2-C5 = O1-C5
 1.2 with sigma of 0.02
4. Restrained planarity
 C4, C5, O1, O2
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
O3 \\sim C15 \\sim O6 \\sim C16 \\sim C14 \\sim O7 \\sim C13 \\sim C17 \\sim O5
\\sim C18 \\sim C12 \\sim O8 \\sim C11 \\sim C19 \\sim O4 \\sim C20 \\sim C10
\\sim C9: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C5 \\sim C1 \\sim N1 \\sim C2 \\sim C3 \\sim C4 \\sim O2 \\sim O1: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02
C8 \\sim C7: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Others
 Fixed Sof: C15(0.5) H15A(0.5) H15B(0.5) O6(0.5) O7(0.5) C1(0.5) H1A(0.5)
 H1B(0.5) C17(0.5) H17A(0.5) H17B(0.5) N1(0.5) H1C(0.5) H1D(0.5) H1E(0.5)
 O8(0.5) C14(0.5) H14A(0.5) H14B(0.5) C16(0.5) H16A(0.5) H16B(0.5) C18(0.5)
 H18A(0.5) H18B(0.5) C19(0.5) H19A(0.5) H19B(0.5) O5(0.5) C9(0.5) H9A(0.5)
 H9B(0.5) O3(0.5) C10(0.5) H10A(0.5) H10B(0.5) C20(0.5) H20A(0.5) H20B(0.5)
 O4(0.5) C11(0.5) H11A(0.5) H11B(0.5) C12(0.5) H12A(0.5) H12B(0.5) C13(0.5)
 H13A(0.5) H13B(0.5) C2(0.5) H2A(0.5) H2B(0.5) C3(0.5) H3A(0.5) H3B(0.5)
 C4(0.5) H4A(0.5) H4B(0.5) O2(0.5) H2(0.5) C5(0.5) O1(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C1(H1A,H1B), C17(H17A,H17B), C14(H14A,H14B), C16(H16A,H16B),
 C18(H18A,H18B), C19(H19A,H19B), C9(H9A,H9B), C10(H10A,H10B), C20(H20A,H20B),
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C2(H2A,H2B), C3(H3A,H3B),
 C4(H4A,H4B)
7.b Tetrahedral OH refined with riding coordinates:
 O2(H2)
7.c Idealised Me refined as rotating group:
 N1(H1C,H1D,H1E)
;
_shelx_res_checksum              15850
_shelx_hkl_checksum              73986
_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
;