Red/green-light emission in continuous dielectric phase transition materials: [Me3NVinyl]2[MnX4] (X = Cl, Br)
Li, Yanyan; Lin, Liting; Yang, Jie; Qian, Kun; Jiang, Tao; Li, Hong; RSC Advances 11 (2021) 2329–2336; doi:10.1039/D0RA08795E

data_7242059
_publ_section_title
;
 Red/green-light emission in continuous dielectric phase transition
 materials: [Me3NVinyl]2[MnX4] (X = Cl, Br)
;
_journal_issue                   4
_journal_name_full               'RSC Advances'
_journal_page_first              2329
_journal_page_last               2336
_journal_paper_doi               10.1039/D0RA08795E
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'Cl4 Mn, 2(C5 H12 N)'
_chemical_formula_sum            'C10 H24 Cl4 Mn N2'
_chemical_formula_weight         369.05
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-07-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-07-31 deposited with the CCDC.	2020-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.224(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.2344(10)
_cell_length_b                   12.6038(4)
_cell_length_c                   18.1345(10)
_cell_measurement_reflns_used    6523
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      75.5030
_cell_measurement_theta_min      10.6670
_cell_volume                     3637.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.957
_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    -25.00  16.00   0.50    0.08    --   46.37 -72.00  92.00   82
  2  \w     25.00  52.00   0.50    0.08    --   46.37 -72.00  92.00   54
  3  \w     36.00  87.00   0.50    0.31    --  107.75 -72.00  92.00  102
  4  \w     71.00 101.00   0.50    0.31    --  107.75 -77.00 120.00   60
  5  \w     76.00 107.00   0.50    0.31    --  107.75-125.00  90.00   62
  6  \w     39.00  65.00   0.50    0.31    --  107.75-125.00  90.00   52
  7  \w     37.00  68.00   0.50    0.31    --  107.75 -61.00   0.00   62
  8  \w     40.00  68.00   0.50    0.31    --  107.75 -61.00 -60.00   56
  9  \w     37.00  67.00   0.50    0.31    --  107.75 -61.00-120.00   60
 10  \w     50.00  95.00   0.50    0.31    --  107.75 -77.00-120.00   90
 11  \w     93.00 157.00   0.50    0.31    --  107.75  15.00   0.00  128
 12  \w    143.00 168.00   0.50    0.31    --  107.75  72.00-137.00   50
 13  \w    100.00 165.00   0.50    0.31    --  107.75  45.00-180.00  130
 14  \w     47.00  72.00   0.50    0.08    --   46.37  72.00-137.00   50
 15  \w    -29.00  22.00   0.50    0.08    --   46.37 -19.00 -60.00  102
 16  \w    -21.00  14.00   0.50    0.08    --   46.37 -19.00  90.00   70
 17  \w     37.00  65.00   0.50    0.31    --  107.75 -61.00 120.00   56
 18  \w    -58.00 -32.00   0.50    0.08    --  -46.37 -72.00  92.00   52
 19  \w   -104.00 -63.00   0.50    0.08    --  -46.37 -72.00  92.00   82
 20  \w    -58.00  27.00   0.50    0.08    --  -46.37  72.00-137.00  170
 21  \w    -54.00 -28.00   0.50    0.31    -- -100.00  45.00 -30.00   52
 22  \w    -53.00 -28.00   0.50    0.31    -- -100.00  45.00  30.00   50
 23  \w    -85.00 -36.00   0.50    0.31    -- -100.00  72.00-137.00   98
 24  \w   -110.00 -83.00   0.50    0.31    -- -100.00 -77.00 -30.00   54
 25  \w   -158.00-119.00   0.50    0.31    -- -100.00 -77.00 -30.00   78
 26  \w   -167.00 -85.00   0.50    0.31    -- -100.00 -72.00  92.00  164
 27  \w   -163.00 -86.00   0.50    0.31    -- -100.00 -30.00 150.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0615506000
_diffrn_orient_matrix_UB_12      -0.0906627000
_diffrn_orient_matrix_UB_13      0.0109350000
_diffrn_orient_matrix_UB_21      0.0613643000
_diffrn_orient_matrix_UB_22      0.0394265000
_diffrn_orient_matrix_UB_23      0.0893483000
_diffrn_orient_matrix_UB_31      -0.0439617000
_diffrn_orient_matrix_UB_32      -0.0717501000
_diffrn_orient_matrix_UB_33      0.0354991000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12898
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         77.257
_diffrn_reflns_theta_min         2.777
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.178
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_preparation       'Magnetic properties,Luminescent'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         12898
_refine_ls_number_restraints     221
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0655
_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^)+(0.0783P)^2^+11.8541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1787
_refine_ls_wR_factor_ref         0.2027
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11061
_reflns_number_total             12898
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9884\% 
 around [1.00 -0.00 0.00] (reciprocal) or [0.90 -0.00 0.44] (direct)
;
_cod_data_source_file            d0ra08795e2.cif
_cod_data_source_block           QK-LYY-200621-CL-200K-AGAIN_twin1_hklf5
_cod_database_code               7242059
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'MnCl4 C4HN'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5019(15)
 0.4981(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N1_1-C5_1
 N1_2-C5_2
 N1_3-C5_3
 N1_4-C5_4
 2.4 with sigma of 0.01
 C4_1-C5_1
 C4_2-C5_2
 C4_3-C5_3
 C4_4-C5_4
 1.34 with sigma of 0.01
 Mn1_5-Cl1_5 \\sim Mn1_5-Cl2_5 \\sim Mn1_5-Cl3_5 \\sim Mn1_5-Cl4_5
 with sigma of 0.02
 Cl1_5-Cl2_5 \\sim Cl2_5-Cl3_5 \\sim Cl1_5-Cl3_5 \\sim Cl1_5-Cl4_5 \\sim
Cl2_5-Cl4_5 \\sim Cl3_5-
 Cl4_5
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1A
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
5. Same fragment restrains
{N1_2, C1_2, C2_2, C3_2, C4_2, C5_2}
{N1_3, C1_3, C2_3, C3_3, C4_3, C5_3}
{N1_4, C1_4, C2_4, C3_4, C4_4, C5_4}
as
{N1_1, C1_1, C2_1, C3_1, C4_1, C5_1} sigma for 1-2: 0.02 1-3: 0.04
6.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C4(H4), C4(H4), C4(H4)
6.b X=CH2 refined with riding coordinates:
 C5(H5A,H5B), C5(H5A,H5B), C5(H5A,H5B), C5(H5A,H5B)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C1(H1A,H1B,H1C), C2(H2A,
 H2B,H2C), C3(H3A,H3B,H3C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C),
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
;
_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 2.331
_oxdiff_exptl_absorpt_empirical_full_min 0.591
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2