Circularly Polarized Luminescence from Chiral Tetranuclear Copper(I) Iodide Clusters.
Yao, Li; Niu, Guangda; Li, Junze; Gao, Liang; Luo, Xufeng; Xia, Bing; Liu, Yuhao; Du, Peipei; Li, Dehui; Chen, Chao; Zheng, Youxuan; Xiao, Zewen; Tang, Jiang; The journal of physical chemistry letters  (2020) 1255–1260; doi:10.1021/acs.jpclett.9b03478

data_8000397
_publ_section_title
;
 Circularly Polarized Luminescence from Chiral Tetranuclear Copper(I)
 Iodide Clusters.
;
_journal_name_full               'The journal of physical chemistry letters'
_journal_page_first              1255
_journal_page_last               1260
_journal_paper_doi               10.1021/acs.jpclett.9b03478
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C32 H44 Cu4 I4 N4'
_chemical_formula_sum            'C32 H44 Cu4 I4 N4'
_chemical_formula_weight         1246.47
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-03-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.54722(4)
_cell_length_b                   12.06809(5)
_cell_length_c                   45.0822(2)
_cell_measurement_reflns_used    79153
_cell_measurement_temperature    294.7(2)
_cell_measurement_theta_max      73.6540
_cell_measurement_theta_min      3.7870
_cell_volume                     4106.11(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.7(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_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    -18.00  58.00   0.50    0.50    --    0.00  19.00   0.00  152
  2  \w    -17.00   8.00   0.50    0.50    --    0.00  38.00 120.00   50
  3  \w    -39.00 -14.00   0.50    0.50    --    0.00 -77.00 120.00   50
  4  \w     41.00  89.00   0.50    0.50    --    0.00  72.00 116.71   96
  5  \w    -10.00  31.00   0.50    0.50    --    0.00 -82.00 -30.00   82
  6  \w    -17.00  60.00   0.50    0.50    --    0.00  19.00  60.00  154
  7  \w    -31.00  22.00   0.50    0.50    --    0.00 -57.00 -90.00  106
  8  \w    -16.00  49.00   0.50    0.50    --    0.00  38.00 150.00  130
  9  \w     48.00  88.00   0.50    0.50    --    0.00  38.00 120.00   80
 10  \w    -15.00  20.00   0.50    0.50    --    0.00  72.00 116.71   70
 11  \w    -89.00 -40.00   0.50    0.50    --    0.00 -57.00 -90.00   98
 12  \w    -12.00  89.00   0.50    0.50    --    0.00  38.00-120.00  202
 13  \w      0.00  29.00   0.50    0.50    --    0.00 -77.00 120.00   58
 14  \w    106.00 164.00   0.50    0.50    --   94.60  63.00  74.75  116
 15  \w     70.00  96.00   0.50    0.50    --   94.60  63.00  74.75   52
 16  \w     72.00 184.00   0.50    0.50    --   94.60  58.00-105.10  224
 17  \w     69.00 100.00   0.50    0.50    --   94.60  66.00 157.80   62
 18  \w     68.00 104.00   0.50    0.50    --   94.60  70.00 112.96   72
 19  \w     72.00 184.00   0.50    0.50    --   94.60  55.00 104.21  224
 20  \w     72.00  97.00   0.50    0.50    --   94.60  56.00-146.81   50
 21  \w     99.00 184.00   0.50    0.50    --   94.60  72.00  48.65  170
 22  \w     67.00  92.00   0.50    0.50    --   94.60  72.00  48.65   50
 23  \w     68.00  93.00   0.50    0.50    --   94.60  70.00  98.34   50
 24  \w     74.00 184.00   0.50    0.50    --   94.60  51.00-157.93  220
 25  \w     71.00  96.00   0.50    0.50    --   94.60  61.00  50.11   50
 26  \w     73.00 131.00   0.50    0.50    --   94.60  52.00  56.63  116
 27  \w     66.00  92.00   0.50    0.50    --   94.60  74.00 137.49   52
 28  \w    123.00 184.00   0.50    0.50    --   94.60  74.00 137.49  122
 29  \w     67.00  92.00   0.50    0.50    --   94.60  73.00-114.20   50
 30  \w     68.00  93.00   0.50    0.50    --   94.60  70.00 -44.09   50
 31  \w     69.00  94.00   0.50    0.50    --   94.60  68.00  -0.62   50
 32  \w     67.00  92.00   0.50    0.50    --   94.60  73.00  15.82   50
 33  \w     72.00 183.00   0.50    0.50    --   94.60  57.00-133.62  222
 34  \w     71.00  96.00   0.50    0.50    --   94.60  65.00 168.53   50
 35  \w    148.00 174.00   0.50    0.50    --   94.60  69.00 -66.48   52
 36  \w     67.00  93.00   0.50    0.50    --   94.60  71.00   1.92   52
 37  \w     68.00  93.00   0.50    0.50    --   94.60  69.00 -81.56   50
 38  \w     70.00  95.00   0.50    0.50    --   94.60  64.00-134.31   50
 39  \w      5.00 124.00   0.50    0.50    --   94.60 -77.00-150.00  238
 40  \w     66.00  91.00   0.50    0.50    --   94.60  75.00 -36.89   50
 41  \w      8.00 125.00   0.50    0.50    --   94.60 -82.00  30.00  234
 42  \w     10.00  36.00   0.50    0.50    --   94.60 -82.00 -60.00   52
 43  \w     44.00 122.00   0.50    0.50    --   94.60 -82.00 -60.00  156
 44  \w     28.00 126.00   0.50    0.50    --   94.60 -82.00 120.00  196
 45  \w     68.00 153.00   0.50    0.50    --   94.60  71.00 123.43  170
 46  \w     32.00 124.00   0.50    0.50    --   94.60 -77.00  60.00  184
 47  \w     71.00  97.00   0.50    0.50    --   94.60  61.00-180.00   52
 48  \w     72.00 183.00   0.50    0.50    --   94.60  57.00 -44.50  222
 49  \w     67.00 110.00   0.50    0.50    --   94.60  73.00 -23.47   86
 50  \w     71.00 182.00   0.50    0.50    --   94.60  61.00   0.00  222
 51  \w     71.00 102.00   0.50    0.50    --   94.60  61.00 150.00   62
 52  \w     72.00 110.00   0.50    0.50    --   94.60  56.00  33.19   76
 53  \w     66.00  91.00   0.50    0.50    --   94.60  75.00-174.02   50
 54  \w     72.00 119.00   0.50    0.50    --   94.60  55.00 -55.74   94
 55  \w    123.00 151.00   0.50    0.50    --   94.60  55.00 -55.74   56
 56  \w     71.00  97.00   0.50    0.50    --   94.60  61.00  60.00   52
 57  \w     69.00  94.00   0.50    0.50    --   94.60  66.00-122.39   50
 58  \w     67.00  92.00   0.50    0.50    --   94.60  71.00-135.92   50
 59  \w     66.00  91.00   0.50    0.50    --   94.60  75.00 -42.38   50
 60  \w     88.00 114.00   0.50    0.50    --   94.60 -82.00-120.00   52
 61  \w     37.00  62.00   0.50    0.50    --   94.60 -82.00-120.00   50
 62  \w     66.00  91.00   0.50    0.50    --   94.60  75.00 -59.04   50
 63  \w     71.00 150.00   0.50    0.50    --   94.60  60.00  89.62  158
 64  \w     68.00  93.00   0.50    0.50    --   94.60  70.00 -96.30   50
 65  \w     72.00 116.00   0.50    0.50    --   94.60  61.00 -90.00   88
 66  \w     68.00  94.00   0.50    0.50    --   94.60  69.00 -66.48   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      -0.0036302000
_diffrn_orient_matrix_UB_12      -0.1162752000
_diffrn_orient_matrix_UB_13      0.0140945000
_diffrn_orient_matrix_UB_21      0.0186170000
_diffrn_orient_matrix_UB_22      0.0522379000
_diffrn_orient_matrix_UB_23      0.0310230000
_diffrn_orient_matrix_UB_31      -0.2032397000
_diffrn_orient_matrix_UB_32      0.0068627000
_diffrn_orient_matrix_UB_33      0.0025925000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            103927
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.945
_diffrn_reflns_theta_min         3.792
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    26.135
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.016
_exptl_crystal_description       needle
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.483
_refine_diff_density_min         -1.247
_refine_diff_density_rms         0.226
_refine_ls_abs_structure_details
;
 Flack x determined using 3380 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         8200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0295
_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^)+(0.0430P)^2^+3.6200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0740
_reflns_Friedel_coverage         0.755
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                8096
_reflns_number_total             8200
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jz9b03478_si_003.cif
_cod_data_source_block           (S-MBA)4Cu4I4
_cod_database_code               8000397
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.623
_shelx_estimated_absorpt_t_min   0.047
_reflns_odcompleteness_completeness 99.86
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2B(H2Ba), C2A(H2Aa), C2C(H2C), C2D(H2D)
2.b Secondary CH2 refined with riding coordinates:
 N2(H2a,H2b), N1(H1a,H1b), N3(H3a,H3b), N4(H4c,H4d)
2.c Aromatic/amide H refined with riding coordinates:
 C6A(H6A), C4A(H4A), C7A(H7A), C5A(H5A), C8A(H8A), C5B(H5B), C8B(H8B),
 C4B(H4B), C7B(H7B), C6B(H6B), C8C(H8C), C4C(H4Ca), C5C(H5C), C7C(H7C),
 C6C(H6C), C4D(H4Da), C8D(H8D), C5D(H5D), C7D(H7D), C6D(H6D)
2.d Idealised Me refined as rotating group:
 C1B(H1Ba,H1Bb,H1Bc), C1A(H1Aa,H1Ab,H1Ac), C1D(H1Da,H1Db,H1Dc), C1C(H1Ca,H1Cb,
 H1Cc)
;
_shelx_res_checksum              396
_shelx_hkl_checksum              13268
_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 18.751
_oxdiff_exptl_absorpt_empirical_full_min 0.456