Room-temperature phosphorescence of manganese-based metal halides
Zhang, Yue; Chen, Dian; Jin, Kai-Hang; Zang, Shuang-Quan; Wang, Qing-Lun; Dalton Transactions  (2021) –; doi:10.1039/D1DT03206B

data_7708693
_publ_section_title
;
 Room-temperature phosphorescence of manganese-based metal halides
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03206B
_journal_year                    2021
_chemical_formula_moiety         'Cl6 Mn, 2(C8 H14 N2)'
_chemical_formula_sum            'C16 H28 Cl6 Mn N4'
_chemical_formula_weight         544.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-17 deposited with the CCDC.	2021-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                101.991(3)
_cell_angle_beta                 99.889(3)
_cell_angle_gamma                112.943(3)
_cell_formula_units_Z            1
_cell_length_a                   7.5206(3)
_cell_length_b                   8.4873(3)
_cell_length_c                   10.5291(3)
_cell_measurement_reflns_used    3780
_cell_measurement_temperature    296.6(6)
_cell_measurement_theta_max      72.7890
_cell_measurement_theta_min      5.9230
_cell_volume                     581.08(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (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      air
_diffrn_ambient_temperature      296.6(6)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.955
_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    -57.00   0.00   0.50    0.50    --    0.00 -38.00  90.00  114
  2  \w    -56.00  12.00   0.50    0.50    --    0.00 -37.00-176.00  136
  3  \w    -13.00  29.00   0.50    0.50    --    0.00 -38.00 -60.00   84
  4  \w    -87.00 -37.00   0.50    0.50    --    0.00 -38.00 -60.00  100
  5  \w      8.00 135.00   0.50    0.50    --   97.60 -82.00   0.00  254
  6  \w      9.00  61.00   0.50    0.50    --   97.60 -61.00-150.00  104
  7  \w    133.00 159.00   0.50    0.50    --   97.60  77.00  60.00   52
  8  \w      8.00 127.00   0.50    0.50    --   97.60 -82.00-150.00  238
  9  \w     92.00 118.00   0.50    0.50    --   97.60 -82.00 120.00   52
 10  \w     64.00 186.00   0.50    0.50    --   97.60  30.00  90.00  244
 11  \w    101.00 130.00   0.50    0.50    --   97.60 -30.00 120.00   58
 12  \w     86.00 123.00   0.50    0.50    --   97.60  45.00 120.00   74
 13  \w     21.00  47.00   0.50    0.50    --   97.60 -30.00 120.00   52
 14  \w     69.00 128.00   0.50    0.50    --   97.60 -61.00-150.00  118
 15  \w     33.00  58.00   0.50    0.50    --   97.60 -82.00 120.00   50
 16  \w    128.00 161.00   0.50    0.50    --   97.60  45.00 120.00   66
 17  \w     71.00 105.00   0.50    0.50    --   97.60  77.00  60.00   68
 18  \w     89.00 114.00   0.50    0.50    --   97.60 -82.00 -90.00   50
 19  \w     65.00 135.00   0.50    0.50    --   97.60 -82.00  60.00  140
 20  \w     98.00 130.00   0.50    0.50    --   97.60  45.00-180.00   64
 21  \w     89.00 115.00   0.50    0.50    --   97.60 -82.00  90.00   52
 22  \w     81.00 183.00   0.50    0.50    --   97.60  61.00 150.00  204
;
_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      0.0169878000
_diffrn_orient_matrix_UB_12      -0.1730990000
_diffrn_orient_matrix_UB_13      0.0074552000
_diffrn_orient_matrix_UB_21      0.2272625000
_diffrn_orient_matrix_UB_22      0.1104245000
_diffrn_orient_matrix_UB_23      0.0694795000
_diffrn_orient_matrix_UB_31      -0.0415583000
_diffrn_orient_matrix_UB_32      0.0242963000
_diffrn_orient_matrix_UB_33      0.1391190000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5478
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4761
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        68.230
_diffrn_reflns_theta_max         73.781
_diffrn_reflns_theta_min         4.490
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.160
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       block
_exptl_crystal_F_000             279
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         2227
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0690P)^2^+0.0868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2139
_reflns_number_total             2227
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03206b2.cif
_cod_data_source_block           2
_cod_original_cell_volume        581.09(3)
_cod_database_code               7708693
_shelx_shelxl_version_number     2016/4
_reflns_odcompleteness_completeness 98.22
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C)
;
_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 3.013
_oxdiff_exptl_absorpt_empirical_full_min 0.643