Heteroleptic mer-[Cr(N^N^N)(CN)3] complexes: synthetic challenge, structural characterization and photophysical properties.
Chong, Julien; Besnard, Céline; Cruz, Carlos M.; Piguet, Claude; Jiménez, Juan Ramón; Dalton Transactions  (2022) –; doi:10.1039/D2DT00126H

data_7709560
_publ_section_title
;
 Heteroleptic mer-[Cr(N^N^N)(CN)3] complexes: synthetic challenge,
 structural characterization and photophysical properties.
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00126H
_journal_year                    2022
_chemical_formula_moiety         'C18 H11 Cr N6'
_chemical_formula_sum            'C18 H11 Cr N6'
_chemical_formula_weight         363.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-10
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2022-01-10 deposited with the CCDC.	2022-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.079(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.09570(10)
_cell_length_b                   13.1460(2)
_cell_length_c                   14.3005(2)
_cell_measurement_reflns_used    65287
_cell_measurement_temperature    119.99(14)
_cell_measurement_theta_max      73.4740
_cell_measurement_theta_min      3.3760
_cell_volume                     1634.53(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.99(14)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_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     18.00  62.00   0.50    1.50    --   32.00  23.00 -94.33   88
  2  \w    -56.00 -28.00   0.50    1.50    --  -40.00 -24.00-122.83   56
  3  \w    -98.00 -22.00   0.50    1.50    --  -53.01 -15.00 -60.00  152
  4  \w    -41.00 -14.00   0.50    1.50    --  -60.50  38.00 158.51   54
  5  \w   -107.00 -38.00   0.50    1.50    --  -60.50 -20.00 169.13  138
  6  \w    -71.00 -45.00   0.50    1.50    --  -60.50 -22.00-152.88   52
  7  \w    -71.00 -45.00   0.50    1.50    --  -60.50 -22.00-131.93   52
  8  \w     29.00  74.00   0.50    1.50    --   66.60 -94.00-150.00   90
  9  \w     32.00  78.00   0.50    1.50    --   69.84 -94.00-150.00   92
 10  \w     32.00  78.00   0.50    1.50    --   69.84 -94.00 -60.00   92
 11  \w     39.00 115.00   0.50    1.50    --   75.25   3.00-112.55  152
 12  \w     57.00 122.00   0.50    1.50    --   75.25  21.00  29.46  130
 13  \w     43.00 121.00   0.50    1.50    --   75.25  17.00-106.17  156
 14  \w     39.00 115.00   0.50    1.50    --   75.25   3.00 -32.06  152
 15  \w     32.00 100.00   0.50    1.50    --   75.25-116.00-162.19  136
 16  \w     34.00  92.00   0.50    1.50    --   75.25-106.00-129.99  116
 17  \w     57.00 122.00   0.50    1.50    --   75.25  21.00 -13.54  130
 18  \w     43.00 121.00   0.50    1.50    --   75.25  18.00 -69.27  156
 19  \w     53.00 122.00   0.50    1.50    --   75.25  20.00  65.88  138
 20  \w     39.00  80.00   0.50    1.50    --   75.25 -89.00 155.41   82
 21  \w     31.00 100.00   0.50    1.50    --   75.25-118.00 -61.08  138
 22  \w     36.00  68.00   0.50    1.50    --   75.25 -68.00 -51.57   64
 23  \w     40.00 116.00   0.50    1.50    --   75.25   5.00-156.74  152
 24  \w     41.00 117.00   0.50    1.50    --   75.25   6.00  38.95  152
 25  \w     48.00 122.00   0.50    1.50    --   75.25  19.00 145.15  148
 26  \w     40.00  76.00   0.50    1.50    --   75.25 -83.00-135.96   72
 27  \w     37.00  85.00   0.50    1.50    --   75.25 -96.00 146.37   96
 28  \w     57.00 122.00   0.50    1.50    --   75.25  21.00-136.42  130
 29  \w     38.00  82.00   0.50    1.50    --   75.25 -93.00 110.82   88
 30  \w     57.00 122.00   0.50    1.50    --   75.25  21.00  96.39  130
 31  \w     35.00  89.00   0.50    1.50    --   75.25-103.00-158.27  108
 32  \w     35.00  90.00   0.50    1.50    --   75.25-104.00 -99.56  110
 33  \w     43.00 119.00   0.50    1.50    --   75.25  11.00 176.94  152
 34  \w     35.00  89.00   0.50    1.50    --   75.25-102.00  14.62  108
 35  \w     24.00  71.00   0.50    1.50    --   40.00  22.00-156.79   94
 36  \w     35.00  95.00   0.50    1.50    --   66.60-125.00 120.00  120
 37  \w     36.00  67.00   0.50    1.50    --   72.00 -74.00  24.18   62
 38  \w      9.00  34.00   0.50    1.50    --    4.00  30.00 -35.65   50
 39  \w      4.00  31.00   0.50    1.50    --   -4.00  33.00 -88.17   54
 40  \w     11.00  37.00   0.50    1.50    --    8.00  29.00-138.52   52
 41  \w      0.00  26.00   0.50    1.50    --   -8.00  33.00-167.19   52
 42  \w     17.00  43.00   0.50    1.50    --   12.00  27.00  90.53   52
 43  \w     19.00  45.00   0.50    1.50    --   20.00  26.00 -12.54   52
 44  \w    -13.00  12.00   0.50    1.50    --  -24.00  47.00  80.78   50
 45  \w     22.00  47.00   0.50    1.50    --   36.00  23.00-122.68   50
 46  \w    -56.00 -31.00   0.50    1.50    --  -40.00 -24.00 131.99   50
 47  \w    -62.00 -37.00   0.50    1.50    --  -48.00 -23.00 -23.87   50
 48  \w    -62.00 -37.00   0.50    1.50    --  -48.00 -23.00  -0.08   50
 49  \w    -60.00 -34.00   0.50    1.50    --  -48.00 -23.00 -95.78   52
 50  \w    -62.00 -36.00   0.50    1.50    --  -48.00 -23.00  24.20   52
 51  \w    -88.00 -20.00   0.50    1.50    --  -53.01   0.00   0.00  136
 52  \w    -62.00 -36.00   0.50    1.50    --  -53.01 125.00-120.00   52
 53  \w    -55.00 -26.00   0.50    1.50    --  -53.01   0.00 150.00   58
 54  \w    -74.00 -48.00   0.50    1.50    --  -53.01 116.00 137.00   52
 55  \w    -65.00 -39.00   0.50    1.50    --  -53.01 125.00 -30.00   52
 56  \w    -84.00 -55.00   0.50    1.50    --  -53.01   0.00-150.00   58
 57  \w    -78.00 -16.00   0.50    1.50    --  -53.01   0.00  60.00  124
 58  \w    -90.00 -63.00   0.50    1.50    --  -53.01   0.00 150.00   54
 59  \w    -41.00 -16.00   0.50    1.50    --  -53.01   0.00-150.00   50
 60  \w    -45.00 -19.00   0.50    1.50    --  -53.01 116.00 137.00   52
 61  \w     44.00  70.00   0.50    1.50    --   60.00  22.00   6.60   52
 62  \w     67.00  94.00   0.50    1.50    --   66.60-125.00 -60.00   54
 63  \w     36.00  78.00   0.50    1.50    --   66.60-125.00   0.00   84
 64  \w     35.00  63.00   0.50    1.50    --   66.60-125.00 -60.00   56
 65  \w     35.00  98.00   0.50    1.50    --   69.84-125.00  90.00  126
 66  \w     66.00  92.00   0.50    1.50    --   69.84-125.00 -30.00   52
 67  \w     36.00  63.00   0.50    1.50    --   69.84-125.00 -30.00   54
 68  \w     73.00  98.00   0.50    1.50    --   69.84-125.00-180.00   50
 69  \w     36.00  62.00   0.50    1.50    --   69.84-125.00-180.00   52
 70  \w     54.00  80.00   0.50    1.50    --   72.66  21.00  88.54   52
 71  \w     53.00  80.00   0.50    1.50    --   75.25  20.00-157.07   54
 72  \w     76.00 102.00   0.50    1.50    --   75.25-121.00 155.11   52
 73  \w     34.00  68.00   0.50    1.50    --   75.25-121.00 155.11   68
 74  \w     37.00  65.00   0.50    1.50    --   75.25 -97.00  89.17   56
 75  \w     34.00  75.00   0.50    1.50    --   75.25-106.00 -83.50   82
 76  \w     35.00  93.00   0.50    1.50    --   75.25-107.00  64.88  116
 77  \w     74.00  99.00   0.50    1.50    --   75.25-115.00  28.11   50
 78  \w     32.00  57.00   0.50    1.50    --   75.25-115.00  28.11   50
 79  \w     40.00  90.00   0.50    1.50    --   75.25-104.00 101.82  100
 80  \w     65.00  94.00   0.50    1.50    --   75.25-110.00 -11.86   58
 81  \w     57.00  92.00   0.50    1.50    --   75.25  21.00 -50.59   70
 82  \w     38.00  64.00   0.50    1.50    --   75.25-110.00 -11.86   52
 83  \w     53.00 117.00   0.50    1.50    --   75.25-150.00  75.70  128
 84  \w     76.00 101.00   0.50    1.50    --   75.25-119.00-109.39   50
 85  \w     88.00 114.00   0.50    1.50    --   75.25   4.00 107.98   52
 86  \w     40.00  76.00   0.50    1.50    --   75.25   4.00 107.98   72
 87  \w     31.00  57.00   0.50    1.50    --   75.25-119.00-109.39   52
 88  \w      9.00  36.00   0.50    1.50    --    4.00  30.00 -35.65   54
 89  \w      4.00  31.00   0.50    1.50    --   -4.00  33.00 -88.17   54
 90  \w      0.00  29.00   0.50    1.50    --   -8.00  34.00  42.90   58
 91  \w     11.00  39.00   0.50    1.50    --    8.00  29.00-138.52   56
 92  \w      0.00  29.00   0.50    1.50    --   -8.00  34.00 121.28   58
 93  \w      8.00  48.00   0.50    1.50    --   12.00  26.00 162.31   80
 94  \w     11.00  44.00   0.50    1.50    --   12.00  27.00  90.53   66
 95  \w     -4.00  23.00   0.50    1.50    --  -16.00  38.00-124.15   54
 96  \w     -4.00  23.00   0.50    1.50    --  -16.00  38.00  99.45   54
 97  \w     -6.00  26.00   0.50    1.50    --  -16.00  36.00   3.79   64
 98  \w     16.00  48.00   0.50    1.50    --   20.00  26.00 -12.54   64
 99  \w    -13.00  13.00   0.50    1.50    --  -24.00  47.00 178.69   52
100  \w    -18.00  19.00   0.50    1.50    --  -28.00  36.00  82.97   74
101  \w    -56.00 -28.00   0.50    1.50    --  -40.00 -24.00 131.99   56
102  \w    -62.00 -34.00   0.50    1.50    --  -48.00 -23.00  12.06   56
103  \w    -62.00 -34.00   0.50    1.50    --  -48.00 -23.00  73.06   56
104  \w    -62.00 -34.00   0.50    1.50    --  -48.00 -23.00 -95.78   56
105  \w    -81.00 -35.00   0.50    1.50    --  -53.01 125.00-120.00   92
106  \w    -90.00 -16.00   0.50    1.50    --  -53.01   0.00  90.00  148
107  \w    -90.00 -16.00   0.50    1.50    --  -53.01   0.00   0.00  148
108  \w    -81.00 -35.00   0.50    1.50    --  -53.01 125.00 -30.00   92
109  \w    -98.00 -22.00   0.50    1.50    --  -53.01 -15.00-180.00  152
110  \w    -70.00 -44.00   0.50    1.50    --  -60.00 -22.00  49.65   52
111  \w     44.00  71.00   0.50    1.50    --   60.00  22.00   6.60   54
112  \w    -71.00 -45.00   0.50    1.50    --  -60.50 -22.00  -9.90   52
113  \w     35.00  95.00   0.50    1.50    --   66.60-125.00 150.00  120
114  \w     29.00  74.00   0.50    1.50    --   66.60 -94.00 -30.00   90
115  \w     35.00  95.00   0.50    1.50    --   66.60-125.00 -90.00  120
116  \w     35.00  95.00   0.50    1.50    --   66.60-125.00-150.00  120
117  \w     33.00 107.00   0.50    1.50    --   69.84   0.00 120.00  148
118  \w     35.00  98.00   0.50    1.50    --   69.84-125.00 120.00  126
119  \w     35.00  98.00   0.50    1.50    --   69.84-125.00   0.00  126
120  \w     32.00  78.00   0.50    1.50    --   69.84 -94.00  30.00   92
121  \w     35.00  98.00   0.50    1.50    --   69.84-125.00-180.00  126
122  \w     35.00  98.00   0.50    1.50    --   69.84-125.00  90.00  126
123  \w     39.00 115.00   0.50    1.50    --   75.25   3.00 -32.06  152
124  \w     39.00 115.00   0.50    1.50    --   75.25   3.00-112.55  152
125  \w     43.00 121.00   0.50    1.50    --   75.25  17.00-106.17  156
126  \w     44.00 120.00   0.50    1.50    --   75.25  14.00  58.06  152
127  \w     37.00  86.00   0.50    1.50    --   75.25 -98.00 141.21   98
128  \w     39.00  71.00   0.50    1.50    --   75.25 -75.00  33.65   64
129  \w     40.00 116.00   0.50    1.50    --   75.25   5.00 164.46  152
130  \w     37.00  85.00   0.50    1.50    --   75.25 -97.00  89.17   96
131  \w     31.00 101.00   0.50    1.50    --   75.25-119.00-109.39  140
132  \w     33.00  96.00   0.50    1.50    --   75.25-111.00 -97.81  126
133  \w     34.00  92.00   0.50    1.50    --   75.25-106.00 -83.50  116
134  \w     53.00 122.00   0.50    1.50    --   75.25  20.00-157.07  138
135  \w     32.00  99.00   0.50    1.50    --   75.25-115.00  28.11  134
136  \w     39.00 114.00   0.50    1.50    --   75.25   2.00  97.58  150
137  \w     32.00 102.00   0.50    1.50    --   75.25-121.00 155.11  140
138  \w     39.00 114.00   0.50    1.50    --   75.25   1.00 162.55  150
139  \w     33.00  95.00   0.50    1.50    --   75.25-110.00 -11.86  124
140  \w     57.00 122.00   0.50    1.50    --   75.25  21.00 -50.59  130
141  \w     43.00 121.00   0.50    1.50    --   75.25  18.00 -69.27  156
142  \w     35.00  90.00   0.50    1.50    --   75.25-104.00 101.82  110
143  \w     34.00  93.00   0.50    1.50    --   75.25-107.00  64.88  118
144  \w     51.00 119.00   0.50    1.50    --   75.25-150.00  75.70  136
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1452500000
_diffrn_orient_matrix_UB_12      0.0566880000
_diffrn_orient_matrix_UB_13      0.0056425000
_diffrn_orient_matrix_UB_21      -0.0720713000
_diffrn_orient_matrix_UB_22      -0.0138923000
_diffrn_orient_matrix_UB_23      -0.1110989000
_diffrn_orient_matrix_UB_31      -0.0714066000
_diffrn_orient_matrix_UB_32      -0.1015810000
_diffrn_orient_matrix_UB_33      0.0183849000
_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  0.0468
_diffrn_reflns_av_unetI/netI     0.0099
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            91918
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.664
_diffrn_reflns_theta_min         4.667
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.864
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.524
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       prism
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.00046(13)
_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   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0539P)^2^+0.6356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0884
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3256
_reflns_number_total             3295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00126h2.cif
_cod_data_source_block           CrtpyCN
_cod_database_code               7709560
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C18 H11 Cr1 N6'
_reflns_odcompleteness_completeness 98.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15)
;
_shelx_res_checksum              43250
_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 1.267
_oxdiff_exptl_absorpt_empirical_full_min 0.839