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_7709559
_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         'C15 H11 Br3 Cr N3'
_chemical_formula_sum            'C15 H11 Br3 Cr N3'
_chemical_formula_weight         525.00
_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             2020-11-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2022-01-10 deposited with the CCDC.	2022-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.309(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4851(2)
_cell_length_b                   14.3395(2)
_cell_length_c                   13.9396(3)
_cell_measurement_reflns_used    21581
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      73.2650
_cell_measurement_theta_min      4.3740
_cell_volume                     1627.81(6)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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      120.00(10)
_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 0.990
_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      2.00  27.00   0.50    1.00    --   -4.00  31.00 175.19   50
  2  \w      9.00  35.00   0.50    1.00    --    4.00  30.00  66.97   52
  3  \w      9.00  34.00   0.50    1.00    --    4.00  30.00-160.76   50
  4  \w     11.00  36.00   0.50    1.00    --    4.00  30.00 132.09   50
  5  \w     -7.00  18.00   0.50    1.00    --  -20.00  39.00 161.17   50
  6  \w    -51.00 -26.00   0.50    1.00    --  -32.00 -25.00 -58.48   50
  7  \w    -28.00   4.00   0.50    1.00    --  -40.00  50.00-116.84   64
  8  \w     29.00  55.00   0.50    1.00    --   40.00  24.00  81.10   52
  9  \w    -61.00 -35.00   0.50    1.00    --  -48.00 -23.00 -47.96   52
 10  \w    -62.00 -36.00   0.50    1.00    --  -48.00 -23.00-105.57   52
 11  \w    -64.00 -39.00   0.50    1.00    --  -53.01 125.00 120.00   50
 12  \w    -66.00 -35.00   0.50    1.00    --  -53.01 125.00-120.00   62
 13  \w    -79.00 -20.00   0.50    1.00    --  -53.01   0.00-150.00  118
 14  \w    -76.00 -42.00   0.50    1.00    --  -53.01 125.00-180.00   68
 15  \w    -70.00 -44.00   0.50    1.00    --  -60.00 -22.00  24.51   52
 16  \w    -96.00 -50.00   0.50    1.00    --  -60.50 -21.00 -61.79   92
 17  \w    -71.00 -46.00   0.50    1.00    --  -60.50 -22.00   3.04   50
 18  \w    -70.00 -45.00   0.50    1.00    --  -60.50 -22.00-122.45   50
 19  \w    -71.00 -46.00   0.50    1.00    --  -60.50 -22.00 -18.26   50
 20  \w     40.00  72.00   0.50    1.00    --   66.60 -94.00  30.00   64
 21  \w     44.00  72.00   0.50    1.00    --   66.60 -94.00  60.00   56
 22  \w     29.00  57.00   0.50    1.00    --   66.60 -94.00-180.00   56
 23  \w     29.00  60.00   0.50    1.00    --   66.60 -94.00-150.00   62
 24  \w     48.00  74.00   0.50    1.00    --   66.60  15.00 -30.00   52
 25  \w     42.00  68.00   0.50    1.00    --   69.84 -94.00 150.00   52
 26  \w     35.00  61.00   0.50    1.00    --   69.84 -94.00   0.00   52
 27  \w     72.00  98.00   0.50    1.00    --   69.84-125.00  90.00   52
 28  \w     46.00  98.00   0.50    1.00    --   69.84   0.00-120.00  104
 29  \w     36.00  61.00   0.50    1.00    --   69.84-125.00   0.00   50
 30  \w     64.00  89.00   0.50    1.00    --   72.66  21.00  72.27   50
 31  \w     88.00 120.00   0.50    1.00    --   75.25  20.00  18.59   64
 32  \w     82.00 107.00   0.50    1.00    --   75.25-131.00 -21.81   50
 33  \w     72.00 100.00   0.50    1.00    --   75.25-116.00  52.74   56
 34  \w     40.00  66.00   0.50    1.00    --   75.25-131.00 -21.81   52
 35  \w     40.00  65.00   0.50    1.00    --   75.25 -63.00  43.55   50
 36  \w     34.00  59.00   0.50    1.00    --   75.25-116.00  52.74   50
 37  \w     86.00 112.00   0.50    1.00    --   75.25  21.00 140.50   52
 38  \w     33.00  65.00   0.50    1.00    --   75.25 -56.00-132.86   64
 39  \w     83.00 112.00   0.50    1.00    --   75.25-139.00 154.45   58
 40  \w     90.00 122.00   0.50    1.00    --   75.25  21.00  57.44   64
 41  \w     46.00  75.00   0.50    1.00    --   75.25 -82.00 -13.96   58
 42  \w     41.00  68.00   0.50    1.00    --   75.25 -97.00  46.19   54
 43  \w     58.00  83.00   0.50    1.00    --   75.25  21.00  57.44   50
 44  \w     58.00  84.00   0.50    1.00    --   75.25  21.00 140.50   52
 45  \w     50.00  82.00   0.50    1.00    --   75.25-135.00 -44.09   64
 46  \w     35.00  60.00   0.50    1.00    --   75.25-103.00 139.20   50
 47  \w     68.00  94.00   0.50    1.00    --   75.25-125.00 -77.59   52
 48  \w     70.00  95.00   0.50    1.00    --   75.25-110.00  23.73   50
 49  \w     57.00  94.00   0.50    1.00    --   75.25  21.00-161.89   74
 50  \w     77.00 102.00   0.50    1.00    --   75.25   4.00-145.35   50
 51  \w     53.00  82.00   0.50    1.00    --   75.25  20.00 -68.52   58
 52  \w     33.00  59.00   0.50    1.00    --   75.25-110.00  23.73   52
 53  \w     42.00  70.00   0.50    1.00    --   75.25   4.00-145.35   56
 54  \w     60.00  87.00   0.50    1.00    --   75.25   0.00-102.71   54
 55  \w     48.00  87.00   0.50    1.00    --   75.25  12.00 -72.19   78
 56  \w     37.00  62.00   0.50    1.00    --   75.25 -96.00 102.71   50
 57  \w     55.00  81.00   0.50    1.00    --   75.25  20.00-170.25   52
 58  \w     52.00 105.00   0.50    1.00    --   75.25   6.00 -35.95  106
 59  \w     60.00  85.00   0.50    1.00    --   75.25  19.00 105.45   50
 60  \w     34.00  62.00   0.50    1.00    --   75.25 -62.00-173.61   56
 61  \w     92.00 117.00   0.50    1.00    --   75.25  21.00 123.04   50
 62  \w     34.00  59.00   0.50    1.00    --   75.25 -61.00  -1.13   50
 63  \w     63.00  89.00   0.50    1.00    --   75.25  21.00  88.14   52
 64  \w     45.00  77.00   0.50    1.00    --   75.25-105.00-133.67   64
 65  \w     61.00  86.00   0.50    1.00    --   75.25  21.00 -25.73   50
 66  \w     35.00  87.00   0.50    1.00    --   75.25-105.00 -12.60  104
 67  \w     58.00  85.00   0.50    1.00    --   75.25  21.00 123.04   54
 68  \w     70.00  95.00   0.50    1.00    --   75.25-112.00  90.94   50
 69  \w     38.00  63.00   0.50    1.00    --   75.25 -92.00 -46.28   50
 70  \w     87.00 112.00   0.50    1.00    --   75.25   1.00 114.33   50
 71  \w     39.00  65.00   0.50    1.00    --   75.25   1.00 114.33   52
 72  \w     63.00  88.00   0.50    1.00    --   75.25-152.00 -19.19   50
 73  \w     35.00  61.00   0.50    1.00    --   75.25-112.00  90.94   52
 74  \w     63.00  90.00   0.50    1.00    --   75.25   7.00  62.35   54
 75  \w     63.00  89.00   0.50    1.00    --   75.25  21.00  25.51   52
;
_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      -0.0388328000
_diffrn_orient_matrix_UB_12      0.0205596000
_diffrn_orient_matrix_UB_13      0.0994642000
_diffrn_orient_matrix_UB_21      0.1847106000
_diffrn_orient_matrix_UB_22      0.0112072000
_diffrn_orient_matrix_UB_23      0.0523468000
_diffrn_orient_matrix_UB_31      -0.0121802000
_diffrn_orient_matrix_UB_32      0.1048397000
_diffrn_orient_matrix_UB_33      -0.0251367000
_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  0.0366
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29627
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.947
_diffrn_reflns_theta_min         4.520
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.393
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.390
_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    2.142
_exptl_crystal_description       block
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0212
_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^)+(0.0294P)^2^+1.5563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0551
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3179
_reflns_number_total             3273
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00126h2.cif
_cod_data_source_block           CrtpyBr
_cod_database_code               7709559
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C15 H11 Cr Br3 N3'
_shelx_estimated_absorpt_t_max   0.539
_shelx_estimated_absorpt_t_min   0.268
_reflns_odcompleteness_completeness 98.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.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              25654
_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 5.987
_oxdiff_exptl_absorpt_empirical_full_min 0.623