One-dimensional organic metal halide nanoribbons with dual emission.
Lee, Sujin; Karkee, Rijan; Ben-Akacha, Azza; Luong, Derek; Vellore Winfred, J. S. Raaj; Lin, Xinsong; Strubbe, David A.; Ma, Biwu; Chemical communications (Cambridge, England) 59 (2023) 3711–3714; doi:10.1039/d3cc00044c

data_7131360
_publ_section_title
;
 One-dimensional organic metal halide nanoribbons with dual emission.
;
_journal_issue                   25
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3711
_journal_page_last               3714
_journal_paper_doi               10.1039/d3cc00044c
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'Cl11 Pb3, H2 O, C8 H28 N5'
_chemical_formula_sum            'C8 H30 Cl11 N5 O Pb3'
_chemical_formula_weight         1223.89
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-24
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2023-02-24 deposited with the CCDC.	2023-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.36620(10)
_cell_length_b                   15.87190(10)
_cell_length_c                   32.1657(2)
_cell_measurement_reflns_used    112230
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      77.3160
_cell_measurement_theta_min      3.8500
_cell_volume                     5802.79(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.978
_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   -120.00 -76.00   0.50    0.33    --  -48.09-143.00 -15.00   88
  2  \w     67.00  96.00   0.50    0.33    --   48.09-127.00 154.00   58
  3  \w     37.00  74.00   0.50    1.32    --  107.75-127.00 154.00   74
  4  \w    103.00 178.00   0.50    1.32    --  107.75  14.00 170.00  150
  5  \w    130.00 156.00   0.50    1.32    --  107.75 114.00 -31.00   52
  6  \w      1.00  26.00   0.50    0.33    --  -48.09  19.00-180.00   50
  7  \w    -17.00  18.00   0.50    0.33    --  -48.09  37.00-150.00   70
  8  \w   -119.00 -85.00   0.50    0.33    --  -48.09 -57.00 150.00   68
  9  \w    -17.00  25.00   0.50    0.33    --  -48.09  37.00-120.00   84
 10  \w     35.00 105.00   0.50    1.32    --  107.75 -94.00-150.00  140
 11  \w     67.00 125.00   0.50    1.32    --  107.75-143.00 -15.00  116
 12  \w     40.00  66.00   0.50    1.32    --  107.75 -45.00-150.00   52
 13  \w     39.00  70.00   0.50    1.32    --  107.75 -45.00 150.00   62
 14  \w     36.00  70.00   0.50    1.32    --  107.75 -45.00  60.00   68
 15  \w     41.00  93.00   0.50    1.32    --  107.75-125.00 -60.00  104
 16  \w     35.00  98.00   0.50    1.32    --  107.75 -94.00-180.00  126
 17  \w     43.00  69.00   0.50    1.32    --  107.75 -45.00  90.00   52
 18  \w     36.00  63.00   0.50    1.32    --  107.75 -45.00  30.00   54
 19  \w     70.00 103.00   0.50    1.32    --  107.75 -94.00-120.00   66
 20  \w    -44.00   9.00   0.50    0.33    --  -48.09  57.00  30.00  106
 21  \w   -115.00 -82.00   0.50    0.33    --  -48.09 -57.00-120.00   66
 22  \w     57.00  94.00   0.50    0.33    --   48.09-125.00 -90.00   74
 23  \w     35.00  87.00   0.50    0.33    --   48.09  56.00 -80.98  104
 24  \w     34.00  61.00   0.50    0.33    --   48.09  56.00  89.65   54
 25  \w     93.00 119.00   0.50    0.33    --   48.09  56.00  67.02   52
 26  \w     76.00 118.00   0.50    0.33    --   48.09  19.00-120.00   84
 27  \w     34.00  67.00   0.50    0.33    --   48.09  54.00 150.52   66
 28  \w     38.00  72.00   0.50    0.33    --   48.09  19.00-120.00   68
 29  \w     91.00 120.00   0.50    0.33    --   48.09  56.00-153.39   58
 30  \w     34.00  65.00   0.50    0.33    --   48.09  56.00  42.44   62
 31  \w     78.00 121.00   0.50    0.33    --   48.09  55.00 173.90   86
 32  \w     76.00 121.00   0.50    0.33    --   48.09  56.00 -23.03   90
 33  \w     36.00 119.00   0.50    0.33    --   48.09  19.00 120.00  166
 34  \w     78.00 104.00   0.50    0.33    --   48.09  56.00-126.75   52
 35  \w     34.00  65.00   0.50    0.33    --   48.09  55.00 173.90   62
 36  \w     34.00  60.00   0.50    0.33    --   48.09  56.00-105.07   52
 37  \w     34.00  75.00   0.50    0.33    --   48.09  56.00 -44.50   82
 38  \w     36.00  63.00   0.50    0.33    --   48.09  56.00 108.32   54
 39  \w     83.00 119.00   0.50    0.33    --   48.09  56.00  15.70   72
 40  \w     34.00  60.00   0.50    0.33    --   48.09  56.00  15.70   52
 41  \w     34.00  63.00   0.50    0.33    --   48.09  56.00-153.39   58
 42  \w     35.00  72.00   0.50    0.33    --   48.09  56.00 -23.03   74
 43  \w     34.00  60.00   0.50    0.33    --   48.09  56.00-126.75   52
 44  \w     35.00  61.00   0.50    0.33    --   48.09  56.00  67.02   52
 45  \w    -98.00 -72.00   0.50    1.32    --  -86.25 -51.00   2.66   52
 46  \w    -98.00 -72.00   0.50    1.32    --  -86.25 -55.00-155.04   52
 47  \w    -98.00 -72.00   0.50    1.32    --  -86.25 -55.00-177.70   52
 48  \w   -113.00 -72.00   0.50    1.32    --  -86.25 -55.00  18.37   82
 49  \w    -98.00 -72.00   0.50    1.32    --  -86.25 -53.00-126.31   52
 50  \w   -120.00 -72.00   0.50    1.32    --  -86.25 -55.00 -70.28   96
 51  \w    -98.00 -72.00   0.50    1.32    --  -86.25 -55.00 -91.63   52
 52  \w    -98.00 -73.00   0.50    1.32    --  -86.25 -50.00  47.07   50
 53  \w   -102.00 -72.00   0.50    1.32    --  -86.25 -51.00 -46.74   60
 54  \w    -97.00 -72.00   0.50    1.32    --  -86.25 -55.00  65.58   50
 55  \w    -97.00 -72.00   0.50    1.32    --  -86.25 -54.00 127.00   50
 56  \w    -97.00 -72.00   0.50    1.32    --  -86.25 -53.00  -9.08   50
 57  \w    -98.00 -72.00   0.50    1.32    --  -86.25 -54.00  75.24   52
 58  \w    -98.00 -72.00   0.50    1.32    --  -86.25 -55.00 105.93   52
 59  \w    -97.00 -72.00   0.50    1.32    --  -86.25 -55.00  87.41   50
 60  \w    -97.00 -72.00   0.50    1.32    --  -86.25 -54.00-115.67   50
 61  \w   -100.00 -74.00   0.50    1.32    --  -86.25 -53.00  29.93   52
 62  \w    -49.00 -23.00   0.50    1.32    --  -86.25  61.00  60.00   52
 63  \w    -98.00 -72.00   0.50    1.32    --  -86.25 -54.00 143.76   52
 64  \w    -97.00 -72.00   0.50    1.32    --  -86.25 -53.00 155.20   50
 65  \w   -149.00-123.00   0.50    1.32    --  -86.25 -55.00 -29.99   52
 66  \w    -99.00 -73.00   0.50    1.32    --  -86.25 -53.00 -52.00   52
 67  \w    -97.00 -72.00   0.50    1.32    --  -86.25 -53.00-146.94   50
 68  \w   -135.00-109.00   0.50    1.32    --  -86.25 -53.00 155.20   52
 69  \w    -97.00 -72.00   0.50    1.32    --  -86.25 -55.00-102.97   50
 70  \w   -159.00-132.00   0.50    1.32    --  -86.25 -55.00-177.70   54
 71  \w    -98.00 -72.00   0.50    1.32    --  -86.25 -53.00  39.96   52
 72  \w    -97.00 -72.00   0.50    1.32    --  -86.25 -54.00-170.76   50
 73  \w    -98.00 -72.00   0.50    1.32    --  -86.25 -55.00 119.61   52
 74  \w    -98.00 -72.00   0.50    1.32    --  -86.25 -51.00 -25.02   52
 75  \w    -98.00 -72.00   0.50    1.32    --  -86.25 -53.00-133.07   52
 76  \w    -98.00 -72.00   0.50    1.32    --  -86.25 -55.00 168.61   52
 77  \w    -98.00 -72.00   0.50    1.32    --  -86.25 -55.00 -83.34   52
 78  \w    -99.00 -72.00   0.50    1.32    --  -86.25 -55.00 -29.99   54
 79  \w     77.00 104.00   0.50    1.32    --  107.75 -94.00  60.00   54
 80  \w     37.00  72.00   0.50    1.32    --  107.75 -94.00  60.00   70
 81  \w    125.00 158.00   0.50    1.32    --  107.75  61.00-120.00   66
 82  \w     91.00 120.00   0.50    1.32    --  107.75  61.00-120.00   58
 83  \w    131.00 163.00   0.50    1.32    --  107.75  45.00-180.00   64
 84  \w     96.00 121.00   0.50    1.32    --  107.75  45.00-180.00   50
 85  \w     36.00 105.00   0.50    1.32    --  107.75 -94.00 150.00  138
 86  \w    128.00 177.00   0.50    1.32    --  107.75  61.00 150.00   98
 87  \w     91.00 123.00   0.50    1.32    --  107.75  61.00 150.00   64
 88  \w    127.00 153.00   0.50    1.32    --  107.75  61.00   0.00   52
 89  \w     39.00  68.00   0.50    1.32    --  107.75-125.00  30.00   58
 90  \w     91.00 121.00   0.50    1.32    --  107.75  61.00   0.00   60
 91  \w     91.00 165.00   0.50    1.32    --  107.75  61.00 -90.00  148
 92  \w    100.00 157.00   0.50    1.32    --  107.75  45.00-150.00  114
 93  \w     96.00 122.00   0.50    1.32    --  107.75  45.00 120.00   52
 94  \w    142.00 168.00   0.50    1.32    --  107.75  45.00  90.00   52
 95  \w     44.00 106.00   0.50    1.32    --  107.75 -94.00 120.00  124
 96  \w     96.00 123.00   0.50    1.32    --  107.75  45.00  90.00   54
 97  \w     91.00 119.00   0.50    1.32    --  107.75  61.00 120.00   56
 98  \w    128.00 178.00   0.50    1.32    --  107.75  61.00  60.00  100
 99  \w     91.00 122.00   0.50    1.32    --  107.75  61.00  60.00   62
100  \w    100.00 154.00   0.50    1.32    --  107.75  45.00-120.00  108
101  \w     46.00  71.00   0.50    1.32    --  107.75 -45.00-180.00   50
102  \w     97.00 148.00   0.50    1.32    --  107.75  45.00 -90.00  102
103  \w     80.00 106.00   0.50    1.32    --  107.75 -94.00  90.00   52
104  \w    127.00 153.00   0.50    1.32    --  107.75  45.00 -30.00   52
105  \w     97.00 126.00   0.50    1.32    --  107.75  45.00 -30.00   58
106  \w     44.00  74.00   0.50    1.32    --  107.75 -94.00  90.00   60
107  \w    101.00 153.00   0.50    1.32    --  107.75  45.00  60.00  104
108  \w     40.00  68.00   0.50    1.32    --  107.75-125.00   0.00   56
109  \w     87.00 112.00   0.50    1.32    --  107.75-125.00   0.00   50
110  \w     81.00 107.00   0.50    1.32    --  107.75-102.00-113.87   52
111  \w     38.00  72.00   0.50    1.32    --  107.75-102.00-113.87   68
112  \w     36.00  61.00   0.50    1.32    --  107.75 -45.00-120.00   50
113  \w     37.00 107.00   0.50    1.32    --  107.75-102.00  51.24  140
114  \w     76.00 106.00   0.50    1.32    --  107.75 -94.00   0.00   60
115  \w     35.00  73.00   0.50    1.32    --  107.75 -94.00   0.00   76
116  \w     95.00 178.00   0.50    1.32    --  107.75  58.00 -11.19  166
117  \w    128.00 176.00   0.50    1.32    --  107.75  61.00-150.00   96
118  \w     91.00 117.00   0.50    1.32    --  107.75  61.00-150.00   52
119  \w    124.00 162.00   0.50    1.32    --  107.75  56.00  26.52   76
120  \w    128.00 154.00   0.50    1.32    --  107.75  45.00 120.00   52
121  \w     96.00 155.00   0.50    1.32    --  107.75  45.00 150.00  118
122  \w    149.00 177.00   0.50    1.32    --  107.75  61.00-180.00   56
123  \w     91.00 120.00   0.50    1.32    --  107.75  61.00-180.00   58
124  \w     93.00 120.00   0.50    1.32    --  107.75  56.00  26.52   54
125  \w     84.00 111.00   0.50    1.32    --  107.75-125.00  30.00   54
126  \w    132.00 165.00   0.50    1.32    --  107.75  61.00 -30.00   66
127  \w     91.00 124.00   0.50    1.32    --  107.75  61.00 -30.00   66
128  \w     48.00  93.00   0.50    1.32    --  107.75 -61.00 -30.00   90
129  \w     70.00 106.00   0.50    1.32    --  107.75 -94.00 -60.00   72
130  \w    143.00 175.00   0.50    1.32    --  107.75  62.00 -77.09   64
131  \w    129.00 177.00   0.50    1.32    --  107.75  61.00  30.00   96
132  \w     92.00 121.00   0.50    1.32    --  107.75  61.00  30.00   58
133  \w     92.00 137.00   0.50    1.32    --  107.75  62.00 -77.09   90
134  \w    145.00 175.00   0.50    1.32    --  107.75  61.00  90.00   60
135  \w     91.00 140.00   0.50    1.32    --  107.75  61.00  90.00   98
136  \w     91.00 178.00   0.50    1.32    --  107.75  61.00 -60.00  174
137  \w     59.00  90.00   0.50    1.32    --  107.75 -61.00 -90.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1323197000
_diffrn_orient_matrix_UB_12      0.0018639000
_diffrn_orient_matrix_UB_13      0.0105034000
_diffrn_orient_matrix_UB_21      -0.0287951000
_diffrn_orient_matrix_UB_22      0.0176804000
_diffrn_orient_matrix_UB_23      -0.0460215000
_diffrn_orient_matrix_UB_31      -0.0079276000
_diffrn_orient_matrix_UB_32      -0.0955243000
_diffrn_orient_matrix_UB_33      -0.0083009000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            70033
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.237
_diffrn_reflns_theta_min         4.764
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    42.731
_exptl_absorpt_correction_T_max  0.292
_exptl_absorpt_correction_T_min  0.016
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.802
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4432
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.063
_refine_diff_density_max         1.508
_refine_diff_density_min         -1.283
_refine_diff_density_rms         0.202
_refine_ls_extinction_coef       0.000047(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         6022
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+23.1008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0956
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5555
_reflns_number_total             6022
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00044c2.cif
_cod_data_source_block           v-4-66-cu-ac_auto
_cod_depositor_comments          'Adding full bibliography for 7131360.cif.'
_cod_original_cell_volume        5802.80(7)
_cod_database_code               7131360
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C8H30Cl11N5OPb3
_chemical_oxdiff_usercomment     150K
_shelx_estimated_absorpt_t_max   0.174
_shelx_estimated_absorpt_t_min   0.041
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, {H1A,H1B,H1C} of N1, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups, {H5A,H5B,H5C} of N5
2. Restrained distances
 H1G-H1B
 2.1 with sigma of 0.02
3.a Free rotating group:
 O1(H1F,H1G)
3.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B), C1(H1D,H1E), C2(H2C,H2D), C3(H3C,H3D),
 C4(H4C,H4D), C5(H5D,H5E), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B)
3.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N5(H5A,H5B,H5C)
;
_shelx_res_checksum              88889
_shelx_hkl_checksum              45524
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.808
_oxdiff_exptl_absorpt_empirical_full_min 0.676