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_8000396
_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                   7.54153(19)
_cell_length_b                   12.0777(4)
_cell_length_c                   45.1161(16)
_cell_measurement_reflns_used    7712
_cell_measurement_temperature    295.65(10)
_cell_measurement_theta_max      73.2120
_cell_measurement_theta_min      3.8320
_cell_volume                     4109.4(2)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.65(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_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    -25.00   2.00   0.50    2.00    --    0.00 -82.00  30.00   54
  2  \w    -33.00  29.00   0.50    2.00    --    0.00 -82.00 -30.00  124
  3  \w    -28.00  27.00   0.50    2.00    --    0.00 -82.00 120.00  110
  4  \w     71.00 139.00   0.50   10.00    --   94.60  61.00  90.00  136
  5  \w      5.00 108.00   0.50   10.00    --   94.60 -61.00 -60.00  206
  6  \w     23.00  68.00   0.50   10.00    --   94.60 -15.00 -60.00   90
  7  \w    103.00 175.00   0.50   10.00    --   94.60  82.00-120.00  144
  8  \w    145.00 171.00   0.50   10.00    --   94.60  61.00  90.00   52
  9  \w     78.00 182.00   0.50   10.00    --   94.60  30.00-180.00  208
 10  \w      6.00 112.00   0.50   10.00    --   94.60 -82.00 -60.00  212
;
_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      -0.0385793000
_diffrn_orient_matrix_UB_12      0.1180720000
_diffrn_orient_matrix_UB_13      -0.0111231000
_diffrn_orient_matrix_UB_21      0.0873137000
_diffrn_orient_matrix_UB_22      -0.0282711000
_diffrn_orient_matrix_UB_23      -0.0299730000
_diffrn_orient_matrix_UB_31      -0.1805251000
_diffrn_orient_matrix_UB_32      -0.0388723000
_diffrn_orient_matrix_UB_33      -0.0121022000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            20862
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.839
_diffrn_reflns_theta_min         3.789
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    26.114
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33438
_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    2.015
_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         0.702
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details
;
 Flack x determined using 2233 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         8036
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0553P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1080
_reflns_Friedel_coverage         0.730
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.946
_reflns_number_gt                6412
_reflns_number_total             8036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jz9b03478_si_002.cif
_cod_data_source_block           (R-MBA)4Cu4I4
_cod_database_code               8000396
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.623
_shelx_estimated_absorpt_t_min   0.047
_reflns_odcompleteness_completeness 99.95
_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:
 C21(H21), C24(H24), C23(H23), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 N2(H2a,H2b), N3(H3a,H3b), N1(H1a,H1b), N4(H4a,H4b)
2.c Aromatic/amide H refined with riding coordinates:
 C51(H51), C81(H81), C41(H41), C71(H71), C61(H61), C84(H84), C44(H44),
 C43(H43), C83(H83), C42(H42), C52(H52), C82(H82), C73(H73), C62(H62), C72(H72),
  C53(H53), C74(H74), C64(H64), C54(H54), C63(H63)
2.d Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C14(H14a,H14b,H14c), C13(H13a,H13b,H13c), C12(H12a,H12b,
 H12c)
;
_shelx_res_checksum              14395
_shelx_hkl_checksum              5761
_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 2.121
_oxdiff_exptl_absorpt_empirical_full_min 0.481