Circularly Polarized Luminescence from Achiral Single Crystals of Hybrid Manganese Halides.
Zhao, Jian; Zhang, Tongjin; Dong, Xi-Yan; Sun, Meng-En; Zhang, Chong; Li, Xinlei; Zhao, Yong Sheng; Zang, Shuang-Quan; Journal of the American Chemical Society 141 (2019) 15755–15760; doi:10.1021/jacs.9b08780

data_4128325
_publ_section_title
;
 Circularly Polarized Luminescence from Achiral Single Crystals of Hybrid
 Manganese Halides.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15755
_journal_page_last               15760
_journal_paper_doi               10.1021/jacs.9b08780
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '0.25(C160 H192 Br16 K8 Mn4 O48)'
_chemical_formula_sum            'C40 H48 Br4 K2 Mn O12'
_chemical_formula_weight         1173.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.650(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.5199(2)
_cell_length_b                   35.8640(7)
_cell_length_c                   27.0516(5)
_cell_measurement_reflns_used    18464
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      73.6810
_cell_measurement_theta_min      2.9710
_cell_volume                     9235.4(3)
_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      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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     45.00  72.00   0.50    2.50    --    0.00  57.00 -30.00   54
  2  \w    -28.00  -3.00   0.50    2.50    --    0.00  77.00 -30.00   50
  3  \w    -18.00  89.00   0.50    2.50    --    0.00  57.00 150.00  214
  4  \w    -62.00 -36.00   0.50    2.50    --    0.00 -82.00 -60.00   52
  5  \w     -3.00  22.00   0.50    2.50    --    0.00  57.00 -30.00   50
  6  \w      1.00  70.00   0.50    2.50    --    0.00  77.00 -30.00  138
  7  \w     -6.00  23.00   0.50    2.50    --    0.00 -82.00 -60.00   58
  8  \w    -88.00  29.00   0.50    2.50    --    0.00 -77.00 120.00  234
  9  \w      8.00 120.00   0.50   15.00    --   95.20 -61.00  60.00  224
 10  \w     73.00 109.00   0.50   15.00    --   95.20 -82.00 -60.00   72
 11  \w      6.00 128.00   0.50   15.00    --   95.20 -82.00  60.00  244
 12  \w      7.00 128.00   0.50   15.00    --   95.20 -82.00-150.00  242
 13  \w      6.00 116.00   0.50   15.00    --   95.20 -61.00-150.00  220
 14  \w     67.00  92.00   0.50   15.00    --   95.20 -30.00 150.00   50
 15  \w    104.00 184.00   0.50   15.00    --   95.20  30.00 -90.00  160
 16  \w     47.00  92.00   0.50   15.00    --   95.20 -45.00  90.00   90
 17  \w     29.00  55.00   0.50   15.00    --   95.20 -30.00 150.00   52
 18  \w     78.00 103.00   0.50   15.00    --   95.20 -82.00   0.00   50
 19  \w     51.00  76.00   0.50   15.00    --   95.20 -82.00   0.00   50
 20  \w     96.00 123.00   0.50   15.00    --   95.20 -82.00-180.00   54
 21  \w     88.00 122.00   0.50   15.00    --   95.20 -82.00 -90.00   68
 22  \w     80.00 179.00   0.50   15.00    --   95.20  30.00 -60.00  198
 23  \w     68.00 154.00   0.50   15.00    --   95.20  15.00  30.00  172
 24  \w     33.00 115.00   0.50   15.00    --   95.20 -30.00 -90.00  164
 25  \w     79.00 104.00   0.50   15.00    --   95.20 -82.00  30.00   50
 26  \w     91.00 116.00   0.50   15.00    --   95.20 -82.00 101.35   50
;
_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      0.0725981000
_diffrn_orient_matrix_UB_12      0.0162328000
_diffrn_orient_matrix_UB_13      0.0464084000
_diffrn_orient_matrix_UB_21      0.0278295000
_diffrn_orient_matrix_UB_22      -0.0397700000
_diffrn_orient_matrix_UB_23      0.0192938000
_diffrn_orient_matrix_UB_31      0.1419269000
_diffrn_orient_matrix_UB_32      -0.0005191000
_diffrn_orient_matrix_UB_33      -0.0267880000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            47205
_diffrn_reflns_point_group_measured_fraction_full 0.765
_diffrn_reflns_point_group_measured_fraction_max 0.765
_diffrn_reflns_theta_full        64.994
_diffrn_reflns_theta_max         64.994
_diffrn_reflns_theta_min         2.464
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.478
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67790
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_description       needle
_exptl_crystal_F_000             4696
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.369
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details
;
 Flack x determined using 2898 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.033(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1063
_refine_ls_number_reflns         12012
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0626
_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^)+(0.0926P)^2^+99.5644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1756
_refine_ls_wR_factor_ref         0.1800
_reflns_Friedel_coverage         0.533
_reflns_Friedel_fraction_full    0.533
_reflns_Friedel_fraction_max     0.533
_reflns_number_gt                10358
_reflns_number_total             12012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08780_si_003.cif
_cod_data_source_block           (KC)2MnBr4
_cod_database_code               4128325
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C H O Mn Br K'
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.484
_shelx_estimated_absorpt_t_min   0.311
_reflns_odcompleteness_completeness 99.67
_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
2. Uiso/Uaniso restraints and constraints
C13 \\sim C14: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C30(H30A,H30B), C7(H7A,H7B), C47(H47A,H47B), C60(H60A,H60B),
 C17(H17A,H17B), C49(H49A,H49B), C57(H57A,H57B), C10(H10A,H10B), C58(H58A,H58B),
  C68(H68A,H68B), C19(H19A,H19B), C70(H70A,H70B), C48(H48A,H48B), C20(H20A,
 H20B), C29(H29A,H29B), C67(H67A,H67B), C9(H9A,H9B), C77(H77A,H77B), C37(H37A,
 H37B), C40(H40A,H40B), C80(H80A,H80B), C78(H78A,H78B), C50(H50A,H50B),
 C27(H27A,H27B), C59(H59A,H59B), C8(H8A,H8B), C28(H28A,H28B), C39(H39A,H39B),
 C69(H69A,H69B), C38(H38A,H38B), C79(H79A,H79B)
3.b Aromatic/amide H refined with riding coordinates:
 C65(H65), C2(H2), C5(H5), C44(H44), C24(H24), C15(H15), C4(H4), C12(H12),
 C45(H45), C43(H43), C64(H64), C33(H33), C54(H54), C52(H52), C25(H25), C72(H72),
  C55(H55), C3(H3), C42(H42), C14(H14), C73(H73), C34(H34), C62(H62), C53(H53),
 C74(H74), C32(H32), C13(H13), C75(H75), C63(H63), C35(H35), C22(H22), C23(H23)
;
_shelx_res_checksum              83688
_shelx_hkl_checksum              23542
_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 1.822
_oxdiff_exptl_absorpt_empirical_full_min 0.643