A series of dynamic single crystals of [MII(en)3]SO4 (M = Ni , Mn, Cd) shows tunable dielectric property and anisotropic thermal expansion
Wu, Cong; Gao, Kaige; Yao, Zi-Shuo; Tao, Jun; Dalton Transactions  (2022) –; doi:10.1039/D2DT00506A

data_7710003
_publ_section_title
;
 A series of dynamic single crystals of [MII(en)3]SO4 (M = Ni , Mn, Cd)
 shows tunable dielectric property and anisotropic thermal expansion
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00506A
_journal_year                    2022
_chemical_formula_moiety         'C6 H24 Mn N6, O4 S'
_chemical_formula_sum            'C6 H24 Mn N6 O4 S'
_chemical_formula_weight         331.31
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-02-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2022-02-15 deposited with the CCDC.	2022-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   15.6935(5)
_cell_length_b                   15.6935(5)
_cell_length_c                   9.5255(4)
_cell_measurement_reflns_used    2966
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.0440
_cell_measurement_theta_min      4.5010
_cell_volume                     2031.69(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.933
_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    -39.00 -13.00   0.50    8.00    --    0.10 -81.00 146.00   52
  2  \w    -89.00   0.00   0.50    8.00    --    0.10 -19.00   0.00  178
  3  \w    -63.00 -38.00   0.50    8.00    --    0.10 -82.00 -90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0398034000
_diffrn_orient_matrix_UB_12      -0.0382873000
_diffrn_orient_matrix_UB_13      0.0374074000
_diffrn_orient_matrix_UB_21      -0.0212794000
_diffrn_orient_matrix_UB_22      0.0303137000
_diffrn_orient_matrix_UB_23      0.0085927000
_diffrn_orient_matrix_UB_31      -0.0261998000
_diffrn_orient_matrix_UB_32      -0.0183924000
_diffrn_orient_matrix_UB_33      -0.0638026000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10980
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.710
_diffrn_reflns_theta_min         3.967
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.147
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1050
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.632
_refine_diff_density_min         -1.267
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1809
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      2.011
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0746P)^2^+3.7126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.1669
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1323
_reflns_number_total             1809
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00506a2.cif
_cod_data_source_block           p-3
_cod_original_cell_volume        2031.69(16)
_cod_database_code               7710003
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.803
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
S1 \\sim O2 \\sim O1: within 2A with sigma of 0.1 and sigma for terminal atoms
of 0.2 within 2A
O1 \\sim S1 \\sim O2: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
Uanis(O1) \\sim Ueq, Uanis(S1) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), N1(H1A,H1B), N2(H2A,H2B), C2(H2C,H2D), C1(H1C,H1D), C3(H3C,H3D)
;
_shelx_res_checksum              38902
_shelx_hkl_checksum              82439
_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 12.268
_oxdiff_exptl_absorpt_empirical_full_min 0.623