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_7708692
_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         'Cl5 Mn, 2(C3 H8 N6), Cl'
_chemical_formula_sum            'C6 H16 Cl6 Mn N12'
_chemical_formula_weight         523.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 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                90
_cell_angle_beta                 93.166(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.40460(10)
_cell_length_b                   15.3969(4)
_cell_length_c                   10.8565(3)
_cell_measurement_reflns_used    3206
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.5100
_cell_measurement_theta_min      2.8570
_cell_volume                     902.03(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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.968
_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     32.00  58.00   0.50    0.50    --    0.00  57.00 -60.00   52
  2  \w    -29.00  17.00   0.50    0.50    --    0.00  38.00-150.00   92
  3  \w     42.00  85.00   0.50    0.50    --    0.00  57.00-120.00   86
  4  \w    -24.00  36.00   0.50    0.50    --    0.00  57.00-120.00  120
  5  \w     94.00 186.00   0.50    0.50    --   98.80  45.00 -60.00  184
  6  \w     41.00 133.00   0.50    0.50    --   98.80 -77.00 -60.00  184
  7  \w     69.00 175.00   0.50    0.50    --   98.80  61.00 -90.00  212
  8  \w     11.00 131.00   0.50    0.50    --   98.80 -82.00  90.00  240
  9  \w     88.00 128.00   0.50    0.50    --   98.80 -82.00 150.00   80
 10  \w     78.00 103.00   0.50    0.50    --   98.80 -45.00 -30.00   50
 11  \w    100.00 126.00   0.50    0.50    --   98.80  45.00-150.00   52
 12  \w      9.00  46.00   0.50    0.50    --   98.80 -45.00 -30.00   74
;
_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      -0.0562024000
_diffrn_orient_matrix_UB_12      0.0980793000
_diffrn_orient_matrix_UB_13      -0.0047106000
_diffrn_orient_matrix_UB_21      -0.2600164000
_diffrn_orient_matrix_UB_22      -0.0174343000
_diffrn_orient_matrix_UB_23      0.0457485000
_diffrn_orient_matrix_UB_31      0.1033511000
_diffrn_orient_matrix_UB_32      0.0094230000
_diffrn_orient_matrix_UB_33      0.1345184000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4101
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.854
_diffrn_reflns_theta_min         4.078
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.338
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40910
_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    1.929
_exptl_crystal_description       block
_exptl_crystal_F_000             526
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.998
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0576
_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^)+(0.1083P)^2^+1.3796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1676
_refine_ls_wR_factor_ref         0.1694
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1736
_reflns_number_total             1849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03206b2.cif
_cod_data_source_block           4
_cod_database_code               7708692
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C N H Cu S'
_chemical_oxdiff_usercomment     ' '
_reflns_odcompleteness_completeness 99.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All N(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3)
2.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N4(H4A,H4B), N5(H5A,H5B)
;
_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 2.095
_oxdiff_exptl_absorpt_empirical_full_min 0.526