Structure and excitation-dependent emission of novel zinc complexes with pyridyltriazoles
Gusev, Alexey; Braga, Elena; Zamnius, Ekaterina; Kiskin, Mikhail; Kryukova, Mariya; Baryshnikova, Alina; Minaev, Boris; Baryshnikov, Gleb; Ågren, Hans; Linert, Wolfgang; RSC Advances 9 (2019) 22143–; doi:10.1039/C9RA02491C

data_7233170
_publ_section_title
;
 Structure and excitation-dependent emission of novel zinc complexes with
 pyridyltriazoles
;
_journal_issue                   38
_journal_name_full               'RSC Advances'
_journal_page_first              22143
_journal_paper_doi               10.1039/C9RA02491C
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C13 H9 Cl2 F N4 Zn'
_chemical_formula_sum            'C13 H9 Cl2 F N4 Zn'
_chemical_formula_weight         376.51
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-05-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-07 deposited with the CCDC.    2019-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                74.608(2)
_cell_angle_beta                 79.912(2)
_cell_angle_gamma                76.548(2)
_cell_formula_units_Z            4
_cell_length_a                   7.2313(2)
_cell_length_b                   14.1852(4)
_cell_length_c                   15.3646(4)
_cell_measurement_reflns_used    10714
_cell_measurement_temperature    116(2)
_cell_measurement_theta_max      72.6810
_cell_measurement_theta_min      6.3220
_cell_volume                     1466.99(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      116(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    -17.00   9.00   0.50    1.05    --   38.95 -99.00  64.00   52
  2  \w     33.00  70.00   0.50    1.05    --   38.95 -99.00  64.00   74
  3  \w     53.00 109.00   0.50    7.22    --  104.92 -99.00  64.00  112
  4  \w    107.00 148.00   0.50    7.22    --  104.92  99.00 170.00   82
  5  \w      0.00  26.00   0.50    1.05    --  -38.95  54.00  90.00   52
  6  \w    -23.00  28.00   0.50    1.05    --  -38.95  77.00-150.00  102
  7  \w    -77.00   0.00   0.50    1.05    --  -38.95 104.00-120.00  154
  8  \w    -58.00 -15.00   0.50    1.05    --  -38.95  54.00  90.00   86
  9  \w   -103.00 -12.00   0.50    1.05    --  -38.95 -77.00  90.00  182
 10  \w    -67.00 -35.00   0.50    1.05    --  -38.95  99.00 170.00   64
 11  \w    -55.00 -30.00   0.50    1.05    --  -38.95 -54.00-180.00   50
 12  \w    -44.00 -18.00   0.50    1.05    --  -38.95 -77.00-150.00   52
 13  \w   -100.00 -68.00   0.50    1.05    --  -38.95 -54.00-180.00   64
 14  \w    -48.00 -13.00   0.50    1.05    --  -38.95 138.00 -30.00   70
 15  \w    -96.00 -54.00   0.50    1.05    --  -38.95 138.00 -30.00   84
 16  \w    -63.00 -37.00   0.50    1.05    --  -38.95  77.00-150.00   52
 17  \w    -85.00 -19.00   0.50    1.05    --  -38.95 -54.00 120.00  132
 18  \w    -75.00 -25.00   0.50    1.05    --  -38.95 104.00-180.00  100
 19  \w    -99.00 -73.00   0.50    1.05    --  -38.95 -65.00 -60.00   52
 20  \w    -43.00 -17.00   0.50    1.05    --  -38.95 -65.00 -60.00   52
 21  \w   -104.00 -56.00   0.50    1.05    --  -38.95 -77.00-150.00   96
 22  \w     -8.00  17.00   0.50    1.05    --  -38.95  99.00 170.00   50
 23  \w    -44.00 -19.00   0.50    1.05    --  -38.95 -21.00 120.00   50
 24  \w   -105.00 -57.00   0.50    1.05    --  -38.95 -21.00 120.00   96
 25  \w     26.00  52.00   0.50    1.05    --   38.95 -77.00   0.00   52
 26  \w     57.00 106.00   0.50    1.05    --   38.95  77.00 -90.00   98
 27  \w     20.00  48.00   0.50    1.05    --   38.95  77.00 -90.00   56
 28  \w    -27.00  15.00   0.50    1.05    --   38.95 -43.00-120.00   84
 29  \w    -22.00  25.00   0.50    1.05    --   38.95 -65.00  90.00   94
 30  \w     46.00  88.00   0.50    1.05    --   38.95-138.00  30.00   84
 31  \w     27.00  52.00   0.50    1.05    --   38.95 -43.00-120.00   50
 32  \w    -25.00  21.00   0.50    1.05    --   38.95 -77.00   0.00   92
 33  \w     18.00  43.00   0.50    1.05    --   38.95-138.00  30.00   50
 34  \w     46.00 103.00   0.50    1.05    --   38.95  32.00  60.00  114
 35  \w     45.00  96.00   0.50    1.05    --   38.95  54.00 150.00  102
 36  \w     87.00 120.00   0.50    7.22    --  104.92 -37.00  90.00   66
 37  \w     39.00  65.00   0.50    7.22    --  104.92 -37.00  90.00   52
 38  \w    129.00 155.00   0.50    7.22    --  104.92  45.00  60.00   52
 39  \w     74.00 100.00   0.50    7.22    --  104.92-133.00   0.00   52
 40  \w     41.00  67.00   0.50    7.22    --  104.92-133.00   0.00   52
 41  \w     41.00 124.00   0.50    7.22    --  104.92-133.00 -90.00  166
 42  \w     41.00 119.00   0.50    7.22    --  104.92 -30.00   0.00  156
 43  \w    100.00 138.00   0.50    7.22    --  104.92  53.00   0.00   76
 44  \w     39.00 114.00   0.50    7.22    --  104.92-111.00  30.00  150
 45  \w     99.00 124.00   0.50    7.22    --  104.92-133.00-150.00   50
 46  \w     42.00  71.00   0.50    7.22    --  104.92-133.00-150.00   58
 47  \w     42.00  95.00   0.50    7.22    --  104.92 -30.00-180.00  106
 48  \w     60.00 127.00   0.50    7.22    --  104.92 -61.00  60.00  134
 49  \w    120.00 146.00   0.50    7.22    --  104.92 111.00  60.00   52
 50  \w     92.00 142.00   0.50    7.22    --  104.92  30.00 120.00  100
 51  \w     99.00 125.00   0.50    7.22    --  104.92-133.00  30.00   52
 52  \w     51.00  77.00   0.50    7.22    --  104.92-133.00  30.00   52
 53  \w     96.00 152.00   0.50    7.22    --  104.92 111.00  90.00  112
 54  \w     67.00 108.00   0.50    7.22    --  104.92-133.00 -60.00   82
 55  \w     41.00 121.00   0.50    7.22    --  104.92 -86.00  90.00  160
 56  \w     49.00  86.00   0.50    7.22    --  104.92 -77.00-180.00   74
 57  \w    112.00 157.00   0.50    7.22    --  104.92  93.00 150.00   90
 58  \w     40.00 123.00   0.50    7.22    --  104.92 -45.00   0.00  166
 59  \w     79.00 153.00   0.50    7.22    --  104.92 133.00   0.00  148
 60  \w     91.00 157.00   0.50    7.22    --  104.92  30.00-150.00  132
 61  \w     81.00 106.00   0.50    7.22    --  104.92  93.00 150.00   50
 62  \w     75.00 100.00   0.50    7.22    --  104.92 -61.00   0.00   50
 63  \w    112.00 150.00   0.50    7.22    --  104.92   7.00   0.00   76
 64  \w     67.00 117.00   0.50    7.22    --  104.92 -77.00 -60.00  100
 65  \w    102.00 127.00   0.50    7.22    --  104.92 -61.00 -90.00   50
 66  \w     57.00 100.00   0.50    7.22    --  104.92   7.00   0.00   86
 67  \w     41.00  93.00   0.50    7.22    --  104.92 -61.00 -90.00  104
 68  \w     98.00 155.00   0.50    7.22    --  104.92  30.00  60.00  114
 69  \w     37.00 106.00   0.50    7.22    --  104.92-111.00 -60.00  138
 70  \w    109.00 134.00   0.50    7.22    --  104.92  30.00  90.00   50
 71  \w     81.00 148.00   0.50    7.22    --  104.92  93.00 120.00  134
 72  \w     80.00 106.00   0.50    7.22    --  104.92  99.00 170.00   52
 73  \w    -44.00 -19.00   0.50    1.05    --    8.00 128.00-106.60   50
 74  \w    -24.00   1.00   0.50    1.05    --   16.00 108.00  42.12   50
 75  \w     -8.00  17.00   0.50    1.05    --   28.00 100.00  -1.98   50
 76  \w    -10.00  15.00   0.50    1.05    --   28.00 104.00  75.74   50
 77  \w     -7.00  18.00   0.50    1.05    --   28.00  99.00-132.80   50
 78  \w     -7.00  18.00   0.50    1.05    --   28.00  99.00 169.94   50
 79  \w     -1.00  24.00   0.50    1.05    --   32.00  93.00-164.82   50
 80  \w     -1.00  24.00   0.50    1.05    --   32.00  93.00 -75.46   50
 81  \w      6.00  31.00   0.50    1.05    --   36.00  87.00 -45.49   50
 82  \w      5.00  30.00   0.50    1.05    --   36.00  89.00  63.94   50
 83  \w      4.00  29.00   0.50    1.05    --   36.00  90.00  -5.30   50
 84  \w      5.00  30.00   0.50    1.05    --   36.00  89.00-157.20   50
 85  \w      5.00  30.00   0.50    1.05    --   36.00  89.00-110.18   50
 86  \w      4.00  29.00   0.50    1.05    --   36.00  90.00 143.89   50
 87  \w     32.00  59.00   0.50    1.05    --   38.95 -54.00  60.00   54
 88  \w     10.00  35.00   0.50    1.05    --   38.95  84.00 -57.10   50
 89  \w     11.00  36.00   0.50    1.05    --   40.00  84.00-141.40   50
 90  \w     11.00  36.00   0.50    1.05    --   40.00  84.00 114.38   50
 91  \w     16.00  41.00   0.50    1.05    --   44.00  82.00-171.45   50
 92  \w     16.00  41.00   0.50    1.05    --   44.00  82.00-100.84   50
 93  \w     16.00  41.00   0.50    1.05    --   44.00  82.00  29.46   50
 94  \w     16.00  41.00   0.50    1.05    --   44.00  82.00   0.36   50
 95  \w     16.00  41.00   0.50    1.05    --   44.00  82.00 -37.52   50
 96  \w     16.00  41.00   0.50    1.05    --   44.00  82.00-141.30   50
 97  \w     16.00  41.00   0.50    1.05    --   44.00  80.00 167.14   50
 98  \w     16.00  41.00   0.50    1.05    --   44.00  82.00  66.11   50
 99  \w     16.00  41.00   0.50    1.05    --   44.00  81.00 142.18   50
100  \w     23.00  49.00   0.50    1.05    --   48.00  76.00 113.46   52
101  \w     28.00  54.00   0.50    1.05    --   52.00  72.00  70.66   52
102  \w     25.00  50.00   0.50    1.05    --   52.00  77.00 -68.52   50
103  \w     25.00  50.00   0.50    1.05    --   52.00  77.00-134.39   50
104  \w     29.00  64.00   0.50    1.05    --   56.00  77.00   5.54   70
105  \w     30.00  55.00   0.50    1.05    --   56.00  75.00 -34.98   50
106  \w     83.00 123.00   0.50    1.05    --   60.00  77.00  78.85   80
107  \w     33.00  58.00   0.50    1.05    --   60.00  77.00  78.85   50
108  \w     33.00  59.00   0.50    1.05    --   60.00  77.00 122.38   52
109  \w     33.00  62.00   0.50    1.05    --   60.00  77.00-105.31   58
110  \w     34.00  60.00   0.50    1.05    --   60.00  76.00  23.79   52
111  \w     34.00  62.00   0.50    1.05    --   60.00  76.00 178.22   56
112  \w     38.00  64.00   0.50    1.05    --   64.00  76.00 138.58   52
113  \w     39.00  65.00   0.50    1.05    --   64.00  76.00  34.78   52
114  \w     37.00  63.00   0.50    1.05    --   64.00  77.00 -87.63   52
115  \w    103.00 129.00   0.50    1.05    --   64.00  76.00  34.78   52
116  \w     41.00  66.00   0.50    1.05    --   68.00  77.00 -54.00   50
117  \w     42.00  80.00   0.50    1.05    --   68.00  75.00-141.74   76
118  \w     44.00  70.00   0.50    1.05    --   68.00  72.00 160.40   52
119  \w     41.00  89.00   0.50    1.05    --   68.00  77.00 -20.69   96
120  \w     43.00  68.00   0.50    1.05    --   68.00  72.00-143.88   50
121  \w     43.00  69.00   0.50    1.05    --   68.00  72.00  88.60   52
122  \w     94.00 128.00   0.50    1.05    --   68.00  77.00 -54.00   68
123  \w     48.00  74.00   0.50    7.22    --   72.00  67.00 126.85   52
124  \w     48.00  74.00   0.50    7.22    --   72.00  72.00 143.39   52
125  \w     47.00  72.00   0.50    7.22    --   72.00  72.00 104.67   50
126  \w     52.00  84.00   0.50    7.22    --   76.00  76.00  -6.98   64
127  \w     50.00  75.00   0.50    7.22    --   76.00  76.00  33.95   50
128  \w     54.00  80.00   0.50    7.22    --   76.00  65.00  71.47   52
129  \w     51.00  77.00   0.50    7.22    --   76.00  73.00-114.71   52
130  \w     53.00  79.00   0.50    7.22    --   76.00  66.00  29.14   52
131  \w     51.00  76.00   0.50    7.22    --   76.00  72.00 175.65   50
132  \w     53.00 117.00   0.50    7.22    --   76.00  68.00-138.91  128
133  \w     51.00  97.00   0.50    7.22    --   76.00  70.00 -38.02   92
134  \w    111.00 145.00   0.50    7.22    --   80.00  71.00 -92.81   68
135  \w     55.00  84.00   0.50    7.22    --   80.00  71.00 -92.81   58
136  \w     54.00  80.00   0.50    7.22    --   80.00  75.00 -74.81   52
137  \w     55.00  81.00   0.50    7.22    --   80.00  73.00  44.94   52
138  \w     58.00  85.00   0.50    7.22    --   84.00  75.00 -21.72   54
139  \w     58.00 100.00   0.50    7.22    --   84.00  76.00-125.66   84
140  \w    124.00 149.00   0.50    7.22    --   84.00  62.00 109.44   50
141  \w     62.00 105.00   0.50    7.22    --   84.00  62.00 109.44   86
142  \w    118.00 144.00   0.50    7.22    --   84.00  65.00-160.80   52
143  \w     61.00  97.00   0.50    7.22    --   84.00  65.00-160.80   72
144  \w     59.00  84.00   0.50    7.22    --   84.00  71.00  27.02   50
145  \w     58.00 137.00   0.50    7.22    --   84.00  75.00 -47.84  158
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1117421000
_diffrn_orient_matrix_UB_12      -0.0497195000
_diffrn_orient_matrix_UB_13      0.0824434000
_diffrn_orient_matrix_UB_21      -0.0616867000
_diffrn_orient_matrix_UB_22      0.0969452000
_diffrn_orient_matrix_UB_23      0.0338412000
_diffrn_orient_matrix_UB_31      -0.1800160000
_diffrn_orient_matrix_UB_32      -0.0364360000
_diffrn_orient_matrix_UB_33      0.0551017000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0104
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10017
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.992
_diffrn_reflns_theta_min         3.005
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.763
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82526
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_description       needle
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.139
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         10017
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0834
_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^)+(0.0923P)^2^+11.8361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2387
_refine_ls_wR_factor_ref         0.2393
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9641
_reflns_number_total             10017
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra02491c2.cif
_cod_data_source_block           11194-ccc-1_twin1_hklf4
_cod_database_code               7233170
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Zn C39 H27 N12 F3 Cl2 '
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6102(18)
 0.3898(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C9A) = Uanis(C14A)
Uanis(C17A) = Uanis(C18A)
Uanis(C13A) = Uanis(C15A)
Uanis(C12A) = Uanis(C16A)
4. Others
 Sof(C14A)=Sof(H14A)=Sof(C16A)=Sof(H16A)=Sof(C15A)=Sof(H15A)=Sof(C18A)=
 Sof(H18A)=1-FVAR(1)
 Sof(C13A)=Sof(H13A)=Sof(C17A)=Sof(H17A)=Sof(C9A)=Sof(H9A)=Sof(C12A)=Sof(H12A)=
 FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 N4A(H4A), N4(H4), C4A(H4AA), C3A(H3A), C6A(H6A), C4(H4B), C5A(H5A), C13(H13),
 C10(H10), C1(H1), C12(H12), C9(H9), C3(H3), C13A(H13A), C2(H2), C17A(H17A),
 C9A(H9A), C12A(H12A), C14A(H14A), C16A(H16A), C15A(H15A), C18A(H18A)
;
_shelx_res_checksum              88863
_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 1.967
_oxdiff_exptl_absorpt_empirical_full_min 0.661
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_twin_special_details
;
Component 2 rotated by -179.9903\% 
 around [-0.00 1.00 0.00] (reciprocal) or [-0.35 0.92 -0.20] (direct)
;