Manganese(II) in Tetrahedral Halide Environment: Factors Governing Bright Green Luminescence
Morad, Viktoriia; Cherniukh, Ihor; Pöttschacher, Lena; Shynkarenko, Yevhen; Yakunin, Sergii; Kovalenko, Maksym V.; Chemistry of Materials  (2019) –; doi:10.1021/acs.chemmater.9b03782

data_4003433
_publ_section_title
;
 Manganese(II) in Tetrahedral Halide Environment: Factors Governing Bright
 Green Luminescence
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.9b03782
_journal_year                    2019
_chemical_formula_moiety         'Cl4 Mn, 2(C10 H22 N)'
_chemical_formula_sum            'C20 H44 Cl4 Mn N2'
_chemical_formula_weight         509.31
_chemical_name_systematic
'N-benzyl-N,N,N-trimethylammonium tetrabromomanganate(II)'
_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     dual
_audit_creation_date             2019-06-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-24 deposited with the CCDC.	2019-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.844(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9617(4)
_cell_length_b                   10.3605(3)
_cell_length_c                   16.6640(4)
_cell_measurement_reflns_used    10632
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.7740
_cell_measurement_theta_min      2.2000
_cell_volume                     2575.39(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28c (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28c (Rigaku OD, 2015)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0839
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.932
_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    -47.00  40.00   1.00   45.00    --   21.49 -57.00 -30.00   87
  2  \w     -7.00  91.00   1.00   45.00    --   21.49  77.00-150.00   98
  3  \w    -25.00  62.00   1.00   45.00    --   21.49 -99.00 -30.00   87
  4  \w    -25.00  62.00   1.00   45.00    --   21.49 -99.00  90.00   87
  5  \w    -49.00  44.00   1.00   45.00    --   21.49 -38.00-180.00   93
  6  \w     -7.00  91.00   1.00   45.00    --   21.49  77.00 -30.00   98
  7  \w      3.00  90.00   1.00   45.00    --   21.49  57.00 120.00   87
  8  \w     34.00  70.00   1.00   45.00    --   21.49 179.00-120.00   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0415326000
_diffrn_orient_matrix_UB_12      0.0241330000
_diffrn_orient_matrix_UB_13      0.0284960000
_diffrn_orient_matrix_UB_21      -0.0222292000
_diffrn_orient_matrix_UB_22      0.0281656000
_diffrn_orient_matrix_UB_23      0.0257148000
_diffrn_orient_matrix_UB_31      0.0064983000
_diffrn_orient_matrix_UB_32      -0.0575624000
_diffrn_orient_matrix_UB_33      0.0245024000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40059
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.982
_diffrn_reflns_theta_min         2.361
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_T_max  0.93985
_exptl_absorpt_correction_T_min  0.93985
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28c (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
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    1.314
_exptl_crystal_description       plate
_exptl_crystal_F_000             1084
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'from acid'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         7638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+0.8961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6639
_reflns_number_total             7638
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm9b03782_si_004.cif
_cod_data_source_block           ic3037
_cod_depositor_comments
;

2020-10-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         407.45
_cod_original_formula_moiety         '0.8(Cl4 Mn), 1.6(C10 H22 N)'
_cod_original_formula_units_Z            5
_cod_original_formula_sum        'C16 H35.20 Cl3.20 Mn0.80 N1.60'
_cod_database_code               4003433
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 N2 H40 Mn Cl4'
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.706
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C008(H00A,H00B), C009(H00C,H00D), C00A(H00W,H00X), C00B(H00E,H00F), C00C(H00Y,
 H), C00D(H00G,H00H), C00E(H00Z,HA), C00F(H00I,H00J), C00G(H00,HB), C00H(H0AA,
 HC), C00I(H1AA,HD), C00J(H00K,H00L), C00K(H2AA,HE), C00L(H3AA,HF), C00M(H00M,
 H00N), C00O(H00R,H00S)
2.b Idealised Me refined as rotating group:
 C00N(H00O,H00P,H00Q), C00P(H4AA,HG,HH), C00Q(H5AA,HI,HJ), C00R(H00T,H00U,H00V)
;
_shelx_res_checksum              74560
_shelx_hkl_checksum              9992
_olex2_date_sample_data_collection 2018-03-21
_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 1.255
_oxdiff_exptl_absorpt_empirical_full_min 0.852
_xtal_radius                     0.2