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_4003434
_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         'I4 Mn, 2(C10 H16 N)'
_chemical_formula_sum            'C20 H32 I4 Mn N2'
_chemical_formula_weight         863.01
_chemical_name_systematic
'N-benzyl-N,N,N-trimethylammonium tetraiodomanganate(II)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.833(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.7389(2)
_cell_length_b                   9.3411(2)
_cell_length_c                   15.7868(3)
_cell_measurement_reflns_used    5800
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      30.6300
_cell_measurement_theta_min      2.5440
_cell_volume                     1431.05(5)
_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      110.00(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 0.889
_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     -8.00  90.25   0.75   25.00    --   21.18  77.00  90.00  131
  2  \w     -8.00  90.25   0.75   25.00    --   21.18  77.00-150.00  131
  3  \w     -7.00  77.00   0.75   25.00    --   21.18  77.00 -90.00  112
  4  \w      7.00  84.25   0.75   25.00    --   21.18  77.00   0.00  103
;
_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      -0.0713748000
_diffrn_orient_matrix_UB_12      0.0162953000
_diffrn_orient_matrix_UB_13      -0.0052770000
_diffrn_orient_matrix_UB_21      -0.0022471000
_diffrn_orient_matrix_UB_22      -0.0222391000
_diffrn_orient_matrix_UB_23      -0.0430392000
_diffrn_orient_matrix_UB_31      -0.0157435000
_diffrn_orient_matrix_UB_32      -0.0707377000
_diffrn_orient_matrix_UB_33      0.0123251000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.889
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12222
_diffrn_reflns_point_group_measured_fraction_full 0.728
_diffrn_reflns_point_group_measured_fraction_max 0.601
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.792
_diffrn_reflns_theta_min         2.099
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.784
_exptl_absorpt_correction_T_max  0.88652
_exptl_absorpt_correction_T_min  0.88652
_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 green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.003
_exptl_crystal_description       needle
_exptl_crystal_F_000             806
_exptl_crystal_recrystallization_method 'Crystallization from hydroiodic acid'
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.12(3)
_refine_ls_extinction_coef       0.00056(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         5391
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+0.4350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0521
_refine_ls_wR_factor_ref         0.0528
_reflns_Friedel_coverage         0.282
_reflns_Friedel_fraction_full    0.418
_reflns_Friedel_fraction_max     0.280
_reflns_number_gt                5227
_reflns_number_total             5391
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm9b03782_si_003.cif
_cod_data_source_block           ica023
_cod_database_code               4003434
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C18 H28 N2 Mn I4'
_chemical_oxdiff_usercomment     ice
_shelx_estimated_absorpt_t_max   0.796
_shelx_estimated_absorpt_t_min   0.114
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. 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
2.a Secondary CH2 refined with riding coordinates:
 C00G(H00U,H00V), C00R(H00O,H00P)
2.b Aromatic/amide H refined with riding coordinates:
 C009(H009), C00B(H00D), C00E(H00T), C00H(H00W), C00I(H00I), C00J(H00J),
 C00L(H00M), C00M(H00N), C00N(H00X), C00O(H00Y)
2.c Idealised Me refined as rotating group:
 C008(H00A,H00B,H00C), C00A(H00Q,H00R,H00S), C00F(H00E,H00F,H00G), C00K(H00H,
 H00K,H00L), C00P(H00Z,H,HA), C00Q(H00,HB,HC)
;
_shelx_res_checksum              94527
_shelx_hkl_checksum              18889
_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 2.079
_oxdiff_exptl_absorpt_empirical_full_min 0.686