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_4128326
_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 Cl16 K8 Mn4 O48)'
_chemical_formula_sum            'C40 H48 Cl4 K2 Mn O12'
_chemical_formula_weight         995.72
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-07-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.0080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.41800(10)
_cell_length_b                   35.5659(3)
_cell_length_c                   26.6416(2)
_cell_measurement_reflns_used    11579
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      72.9780
_cell_measurement_theta_min      2.9790
_cell_volume                     8922.48(14)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_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    -29.00  69.00   0.50    0.58    --    0.00  38.00 -90.00  196
  2  \w    -15.00  22.00   0.50    0.58    --    0.00  38.00-180.00   74
  3  \w     47.00  88.00   0.50    0.58    --    0.00  38.00-180.00   82
  4  \w     95.00 172.00   0.50    5.00    --   97.60  45.00-120.00  154
  5  \w     10.00 126.00   0.50    5.00    --   97.60 -77.00 -60.00  232
  6  \w      8.00 124.00   0.50    5.00    --   97.60 -61.00-180.00  232
  7  \w     65.00 175.00   0.50    5.00    --   97.60  30.00  30.00  220
  8  \w     71.00  97.00   0.50    5.00    --   97.60  45.00-180.00   52
  9  \w    153.00 178.00   0.50    5.00    --   97.60  45.00-180.00   50
 10  \w     28.00 121.00   0.50    5.00    --   97.60 -82.00-180.00  186
;
_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      0.0965244000
_diffrn_orient_matrix_UB_12      -0.0212651000
_diffrn_orient_matrix_UB_13      -0.0364558000
_diffrn_orient_matrix_UB_21      -0.1127193000
_diffrn_orient_matrix_UB_22      0.0047495000
_diffrn_orient_matrix_UB_23      -0.0421415000
_diffrn_orient_matrix_UB_31      0.0690619000
_diffrn_orient_matrix_UB_32      0.0374450000
_diffrn_orient_matrix_UB_33      -0.0153446000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            20464
_diffrn_reflns_point_group_measured_fraction_full 0.782
_diffrn_reflns_point_group_measured_fraction_max 0.782
_diffrn_reflns_theta_full        65.047
_diffrn_reflns_theta_max         65.047
_diffrn_reflns_theta_min         2.988
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.782
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62725
_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            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       needle
_exptl_crystal_F_000             4120
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 3590 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1198
_refine_ls_number_reflns         11866
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0387P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0747
_reflns_Friedel_coverage         0.566
_reflns_Friedel_fraction_full    0.566
_reflns_Friedel_fraction_max     0.566
_reflns_number_gt                11045
_reflns_number_total             11866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08780_si_002.cif
_cod_data_source_block           (KC)2MnCl4
_cod_database_code               4128326
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.550
_shelx_estimated_absorpt_t_min   0.344
_reflns_odcompleteness_completeness 99.65
_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.a Secondary CH2 refined with riding coordinates:
 C9(H95,H96), C15(H6,H5), C18(H54,H53), C22(H11,H12), C26(H59,H60), C31(H71,
 H72), C38(H24,H23), C39(H47,H48), C40(H42,H41), C46(H89,H90), C53(H18,H17),
 C57(H66,H65), C62(H78,H77), C69(H35,H36), C71(H83,H84)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H16), C2(H1), C6(H2), C7(H73), C8(H49), C12(H61), C14(H52), C16(H3),
 C17(H51), C19(H40), C27(H13), C29(H4), C37(H50), C41(H63), C42(H62), C43(H74),
 C48(H26), C49(H15), C54(H14), C56(H25), C59(H39), C60(H88), C61(H38), C63(H64),
  C65(H87), C66(H37), C67(H75), C70(H76), C72(H86), C76(H28), C77(H85), C79(H27)
;
_shelx_res_checksum              69423
_shelx_hkl_checksum              95420
_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 1.395
_oxdiff_exptl_absorpt_empirical_full_min 0.724