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_7710590
_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         'C6 Cr Mn O12, C12 H24 O6, C5 H12 N O2, C H4 O'
_chemical_formula_sum            'C24 H40 Cr Mn N O21'
_chemical_formula_weight         785.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 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                 94.612(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2411(3)
_cell_length_b                   16.5508(4)
_cell_length_c                   22.7081(8)
_cell_measurement_reflns_used    11525
_cell_measurement_temperature    273.0(2)
_cell_measurement_theta_max      31.2620
_cell_measurement_theta_min      2.4440
_cell_volume                     3461.90(19)
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_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_environment      N~2~
_diffrn_ambient_temperature      273.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.838
_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     -2.00  67.00   0.50    7.63    --   -4.89  41.00 -31.00  138
  2  \w    -70.00 -10.00   0.50    7.63    --   -4.89 -41.00 176.00  120
  3  \w     -9.00  26.00   0.50    7.63    --   -4.89 -99.00 120.00   70
  4  \w     -6.00  23.00   0.50    7.63    --   -4.89 -99.00  60.00   58
  5  \w    -17.00  23.00   0.50    7.63    --   -4.89 -99.00 150.00   80
  6  \w    -16.00  26.00   0.50    7.63    --   -4.89 -99.00-120.00   84
  7  \w    -15.00  10.00   0.50    7.63    --    5.13 -99.00 120.00   50
  8  \w    -68.00  17.00   0.50    7.63    --    5.13 -37.00  60.00  170
  9  \w     -6.00  46.00   0.50    7.63    --    5.13  19.00  90.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0056611000
_diffrn_orient_matrix_UB_12      -0.0062193000
_diffrn_orient_matrix_UB_13      0.0306242000
_diffrn_orient_matrix_UB_21      -0.0658587000
_diffrn_orient_matrix_UB_22      -0.0214123000
_diffrn_orient_matrix_UB_23      -0.0064702000
_diffrn_orient_matrix_UB_31      0.0395182000
_diffrn_orient_matrix_UB_32      -0.0365957000
_diffrn_orient_matrix_UB_33      -0.0014809000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.838
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            25801
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.838
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.997
_diffrn_reflns_theta_min         2.461
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64955
_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    1.507
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.14(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         7458
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0377P)^2^+10.5184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1308
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.838
_reflns_number_gt                6071
_reflns_number_total             7458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01615j2.cif
_cod_data_source_block           valeric18c6_auto
_cod_original_cell_volume        3461.92(17)
_cod_database_code               7710590
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         CHOMnCrN
_chemical_oxdiff_usercomment     223K
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.928
_diffrn_oxdiff_digest_frames
;
0174aa27004b272245b06eaa8f8ec0aa4b00025c89f
;
_diffrn_oxdiff_digest_hkl
;
01821e787d0f6ce62c73a77b62e3e6bd88afe8
;
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.86(3)
 0.14(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Restrained distances
 C3A-C4 = C3B-C4 = C3B-C2B = C3A-C2A = C2A-C1 = C2B-C1
 1.52 with sigma of 0.02
 O2A-C5 = O2B-C5
 1.15 with sigma of 0.02
 O2B-C5
 1.25 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O2B \\sim O2A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
5. Others
 Sof(H1BC)=Sof(H1BD)=Sof(H4BC)=Sof(H4BD)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(C2B)=
 Sof(H2BA)=Sof(H2BB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H4AA)=Sof(H4AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=
 Sof(H3AA)=Sof(H3AB)=FVAR(1)
 Sof(O2B)=Sof(H2B)=1-FVAR(2)
 Sof(O2A)=Sof(H2A)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C17(H17A,H17B), C15(H15A,H15B), C16(H16A,H16B), C23(H23A,
 H23B), C20(H20A,H20B), C14(H14A,H14B), C13(H13A,H13B), C24(H24A,H24B),
 C18(H18A,H18B), C21(H21A,H21B), C19(H19A,H19B), C1(H1AA,H1AB), C1(H1BC,H1BD),
 C4(H4AA,H4AB), C4(H4BC,H4BD), C2A(H2AA,H2AB), C3A(H3AA,H3AB), C3B(H3BA,H3BB),
 C2B(H2BA,H2BB)
6.b Tetrahedral OH refined with riding coordinates:
 O3(H3), O2A(H2A), O2B(H2B)
6.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              507
_shelx_hkl_checksum              15834
_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 1.322
_oxdiff_exptl_absorpt_empirical_full_min 0.817