Promoting structural distortion to enhance the crystal field strength of Mn(II) in tetrahedral bromide for near-unity yellow emission.
Qi, Zhikai; Zhang, Ke; Zhao, Xingxing; Zhang, Nan; Li, Shi-Li; Zhang, Xian-Ming; Chemical communications (Cambridge, England) 60 (2024) 12880–12883; doi:10.1039/d4cc04300f

data_7133836
_publ_section_title
;
 Promoting structural distortion to enhance the crystal field strength of
 Mn(II) in tetrahedral bromide for near-unity yellow emission.
;
_journal_issue                   88
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12880
_journal_page_last               12883
_journal_paper_doi               10.1039/d4cc04300f
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         '2(Br4 Mn), 4(C7 H11 N2)'
_chemical_formula_sum            'C28 H44 Br8 Mn2 N8'
_chemical_formula_weight         1241.87
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-08-07 deposited with the CCDC.	2024-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.1106(6)
_cell_length_b                   16.5169(3)
_cell_length_c                   7.9113(2)
_cell_measurement_reflns_used    15148
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.7770
_cell_measurement_theta_min      3.3770
_cell_volume                     4326.57(16)
_computing_cell_refinement       'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0251
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -39.00   8.00   1.00   27.69    --  -18.34 -77.00-150.00   47
  2  \w    -39.00   8.00   1.00   27.69    --  -18.34 -77.00  60.00   47
  3  \w    -35.00  49.00   1.00   27.69    --  -18.34  57.00 150.00   84
  4  \w    -39.00   8.00   1.00   27.69    --  -18.34 -77.00   0.00   47
  5  \w    -39.00   8.00   1.00   27.69    --  -18.34 -77.00-120.00   47
  6  \w    -39.00   8.00   1.00   27.69    --  -18.34 -77.00 150.00   47
  7  \w    -88.00  51.00   1.00   27.69    --  -18.34   0.00 -30.00  139
  8  \w    -35.00  49.00   1.00   27.69    --  -18.34  57.00   0.00   84
  9  \w    -45.00  -8.00   1.00   27.69    --  -18.34  77.00  60.00   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0101771000
_diffrn_orient_matrix_UB_12      0.0000693000
_diffrn_orient_matrix_UB_13      0.0788828000
_diffrn_orient_matrix_UB_21      -0.0160660000
_diffrn_orient_matrix_UB_22      0.0224818000
_diffrn_orient_matrix_UB_23      0.0362624000
_diffrn_orient_matrix_UB_31      -0.0098569000
_diffrn_orient_matrix_UB_32      -0.0365832000
_diffrn_orient_matrix_UB_33      0.0224463000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            53087
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.854
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.001
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.92a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.907
_exptl_crystal_description       block
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 2243 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         8841
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+0.9883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0670
_reflns_Friedel_coverage         0.777
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6450
_reflns_number_total             8841
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04300f2.cif
_cod_data_source_block           (DMPAH)2MnBr4
_cod_depositor_comments          'Adding full bibliography for 7133836.cif.'
_cod_database_code               7133836
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.502
_shelx_estimated_absorpt_t_min   0.502
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N6(H6A), N4(H4), N8(H8), C21(H21), C25(H25), C28(H28), C7(H7),
 C14(H14), C11(H11), C6(H6), C20(H20), C13(H13), C12(H12), C4(H4A), C18(H18),
 C5(H5), C26(H26), C19(H19), C27(H27)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C16(H16A,H16B,H16C), C22(H22A,H22B,H22C), C1(H1A,H1B,H1C),
 C9(H9A,H9B,H9C), C15(H15A,H15B,H15C), C8(H8A,H8B,H8C), C23(H23A,H23B,H23C)
;
_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 1.707
_oxdiff_exptl_absorpt_empirical_full_min 0.818