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_4003432
_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         'Br4 Mn, 2(C6 H15 Br N)'
_chemical_formula_sum            'C12 H30 Br6 Mn N2'
_chemical_formula_weight         736.78
_chemical_name_systematic
'2-bromo-N,N,N-trimethylethan-1-aminium tetrabromomanganate(II)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 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                 91.653(3)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   23.5987(8)
_cell_length_b                   9.4951(2)
_cell_length_c                   15.7871(5)
_cell_measurement_reflns_used    6578
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      30.7730
_cell_measurement_theta_min      2.4590
_cell_volume                     3535.98(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.23a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.23a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.23a (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      150.01(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 0.923
_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    -63.00  47.00   1.00   25.00    --  -25.15  19.00 -30.00  110
  2  \w    -88.00 -62.00   1.00   25.00    --  -25.15 138.00 -58.00   26
  3  \w    -94.00  -7.00   1.00   25.00    --  -25.15 -57.00 150.00   87
  4  \w    -38.00  40.00   1.00   25.00    --  -25.15  57.00  30.00   78
  5  \w    -90.00 -64.00   1.00   25.00    --  -25.15 -57.00 120.00   26
  6  \w     61.00  89.00   1.00   25.00    --   25.62-138.00-121.00   28
  7  \w      3.00  62.00   1.00   25.00    --   25.62 -99.00  90.00   59
  8  \w     23.00  64.00   1.00   25.00    --   25.62 -99.00 -60.00   41
;
_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      0.0002144000
_diffrn_orient_matrix_UB_12      0.0005672000
_diffrn_orient_matrix_UB_13      -0.0449386000
_diffrn_orient_matrix_UB_21      0.0300474000
_diffrn_orient_matrix_UB_22      -0.0016926000
_diffrn_orient_matrix_UB_23      0.0015961000
_diffrn_orient_matrix_UB_31      -0.0006993000
_diffrn_orient_matrix_UB_32      -0.0746822000
_diffrn_orient_matrix_UB_33      -0.0003520000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.0878
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            40840
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.670
_diffrn_reflns_theta_min         2.145
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.727
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.23a (Rigaku Oxford Diffraction, 2015)
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    2.076
_exptl_crystal_description       block
_exptl_crystal_F_000             2106
_exptl_crystal_recrystallization_method 'Crystallized from ethanol'
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.014
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       0.00019(2)
_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   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         11983
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0577
_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^)+(0.0145P)^2^+0.6999P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0813
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8033
_reflns_number_total             11983
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm9b03782_si_001.cif
_cod_data_source_block           1
_cod_database_code               4003432
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H40 P2 Mn Br6'
_shelx_estimated_absorpt_t_max   0.223
_shelx_estimated_absorpt_t_min   0.042
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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:
 C00F(H00P,H00Q), C00H(H00D,H00E), C00J(H00I,H00J), C00K(H00K,H00L), C00L(H00R,
 H00S), C00M(H00T,H00U), C00Q(H1AA,HD), C00S(H3AA,HG), C00V(H4AA,HJ)
2.b Idealised Me refined as rotating group:
 C00G(H00A,H00B,H00C), C00I(H00F,H00G,H00H), C00N(H00M,H00N,H00O), C00O(H00,H,
 HA), C00P(H0AA,HB,HC), C00R(H2AA,HE,HF), C00T(H00V,H00W,H00X), C00U(H00Y,HH,
 HI), C00W(H00Z,HK,HL)
;
_shelx_res_checksum              85535
_shelx_hkl_checksum              59419
_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 2.104
_oxdiff_exptl_absorpt_empirical_full_min 0.692