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_7710002
_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 N6 Ni1, O4 S0.981'
_chemical_formula_sum            'C6 H24 N6 Ni O4 S0.98'
_chemical_formula_weight         334.44
_space_group_crystal_system      trigonal
_space_group_IT_number           163
_space_group_name_Hall           '-P 3 2c'
_space_group_name_H-M_alt        'P -3 1 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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            2
_cell_length_a                   8.9389(5)
_cell_length_b                   8.9389(5)
_cell_length_c                   9.6152(5)
_cell_measurement_reflns_used    1708
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5740
_cell_measurement_theta_min      4.5550
_cell_volume                     665.36(6)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.884
_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    -89.00 -53.00   0.50    0.88    --    0.10 -63.00  52.00   72
  2  \w    -59.00  -9.00   0.50    0.88    --    0.10 -82.00 150.00  100
  3  \w     -8.00  27.00   0.50    0.88    --    0.10 -82.00   0.00   70
;
_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      -0.0507390000
_diffrn_orient_matrix_UB_12      0.0339329000
_diffrn_orient_matrix_UB_13      0.0271229000
_diffrn_orient_matrix_UB_21      -0.0250067000
_diffrn_orient_matrix_UB_22      -0.0585007000
_diffrn_orient_matrix_UB_23      0.0566294000
_diffrn_orient_matrix_UB_31      0.0720722000
_diffrn_orient_matrix_UB_32      0.0618091000
_diffrn_orient_matrix_UB_33      0.0387230000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3110
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.748
_diffrn_reflns_theta_min         4.239
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.630
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83296
_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 violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             355
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0362P)^2^+0.3811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0764
_reflns_Friedel_coverage         0.000
_reflns_number_gt                539
_reflns_number_total             573
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00506a2.cif
_cod_data_source_block           p-31c
_cod_original_cell_volume        665.36(8)
_cod_database_code               7710002
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.42
_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. Rigid body (RIGU) restrains
 O2, O1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Others
 Fixed Sof: O1(0.33333) O2(0.33333)
4.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D)
;
_shelx_res_checksum              78031
_shelx_hkl_checksum              34382
_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 1.391
_oxdiff_exptl_absorpt_empirical_full_min 0.867