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_7708691
_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(C4 H9 N5)'
_chemical_formula_sum            'C8 H18 Cl6 Mn N10'
_chemical_formula_weight         521.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/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                 105.229(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9461(3)
_cell_length_b                   9.6604(3)
_cell_length_c                   11.2084(3)
_cell_measurement_reflns_used    1069
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      72.4100
_cell_measurement_theta_min      5.6430
_cell_volume                     934.65(5)
_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      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.962
_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     62.00  87.00   0.50    0.50    --    0.00  57.00-180.00   50
  2  \w    -23.00  27.00   0.50    0.50    --    0.00  38.00-120.00  100
  3  \w    -28.00  -2.00   0.50    0.50    --    0.00  57.00-180.00   52
  4  \w     53.00  81.00   0.50    0.50    --    0.00  38.00-120.00   56
  5  \w     63.00 187.00   0.50    0.70    --   97.60  77.00 -60.00  248
  6  \w     80.00 135.00   0.50    0.70    --   97.60  77.00   0.00  110
  7  \w     95.00 187.00   0.50    0.70    --   97.60  61.00-120.00  184
  8  \w     64.00 129.00   0.50    0.70    --   97.60 -82.00  90.00  130
  9  \w    139.00 181.00   0.50    0.70    --   97.60  77.00   0.00   84
 10  \w     10.00  74.00   0.50    0.70    --   97.60 -77.00  90.00  128
 11  \w     77.00 103.00   0.50    0.70    --   97.60  45.00-120.00   52
 12  \w     77.00 103.00   0.50    0.70    --   97.60  61.00 150.00   52
;
_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      -0.0841774000
_diffrn_orient_matrix_UB_12      -0.1356628000
_diffrn_orient_matrix_UB_13      -0.0491084000
_diffrn_orient_matrix_UB_21      -0.0989806000
_diffrn_orient_matrix_UB_22      0.0777110000
_diffrn_orient_matrix_UB_23      -0.1134670000
_diffrn_orient_matrix_UB_31      0.1224475000
_diffrn_orient_matrix_UB_32      -0.0306774000
_diffrn_orient_matrix_UB_33      -0.0709000000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1961
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.220
_diffrn_reflns_theta_min         5.656
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.802
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51266
_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    1.855
_exptl_crystal_description       block
_exptl_crystal_F_000             526
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         963
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0750P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1031
_reflns_Friedel_coverage         0.000
_reflns_number_gt                907
_reflns_number_total             963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03206b2.cif
_cod_data_source_block           3
_cod_database_code               7708691
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.545
_shelx_estimated_absorpt_t_min   0.445
_reflns_odcompleteness_completeness 99.78
_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 N(H) groups, All N(H,H) groups
2. Others
 Fixed Sof: H3A(0.5) H3B(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3)
3.b X=CH2 refined with riding coordinates:
 N2(H2A,H2B), N3(H3A,H3B)
;
_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 1.695
_oxdiff_exptl_absorpt_empirical_full_min 0.675