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_7709558
_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         'C26 H15 Cr N6, 3.277(H2 O)'
_chemical_formula_sum            'C26 H21.55 Cr N6 O3.28'
_chemical_formula_weight         522.45
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-05-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-01-10 deposited with the CCDC.	2022-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                67.150(2)
_cell_angle_beta                 76.292(2)
_cell_angle_gamma                85.697(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1680(3)
_cell_length_b                   10.6947(2)
_cell_length_c                   12.3560(3)
_cell_measurement_reflns_used    17910
_cell_measurement_temperature    120.00(14)
_cell_measurement_theta_max      72.9280
_cell_measurement_theta_min      3.9390
_cell_volume                     1202.71(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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(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 0.995
_diffrn_measured_fraction_theta_max 0.974
_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      9.00  34.00   0.50    2.00    --    4.00  30.00 163.34   50
  2  \w      6.00  32.00   0.50    2.00    --    4.00  28.00 -16.56   52
  3  \w     12.00  38.00   0.50    2.00    --    4.00  29.00 105.77   52
  4  \w      4.00  29.00   0.50    2.00    --   -4.00  33.00-117.32   50
  5  \w     11.00  36.00   0.50    2.00    --    8.00  29.00  53.02   50
  6  \w     15.00  40.00   0.50    2.00    --   16.00  27.00-178.93   50
  7  \w     18.00  45.00   0.50    2.00    --   20.00  26.00  66.21   54
  8  \w     24.00  50.00   0.50    2.00    --   24.00  25.00   9.98   52
  9  \w    -51.00 -26.00   0.50    2.00    --  -32.00 -25.00 103.55   50
 10  \w    -51.00 -26.00   0.50    2.00    --  -32.00 -25.00   9.56   50
 11  \w    -21.00   5.00   0.50    2.00    --  -32.00  57.00  90.28   52
 12  \w    -51.00 -24.00   0.50    2.00    --  -32.00 -25.00 -57.83   54
 13  \w    -20.00   8.00   0.50    2.00    --  -36.00  51.00-116.09   56
 14  \w    -56.00 -31.00   0.50    2.00    --  -40.00 -24.00 -35.98   50
 15  \w    -56.00 -30.00   0.50    2.00    --  -40.00 -24.00 -90.98   52
 16  \w    -62.00 -37.00   0.50    2.00    --  -48.00 -23.00 137.77   50
 17  \w    -61.00 -35.00   0.50    2.00    --  -48.00 -23.00  41.51   52
 18  \w    -61.00 -36.00   0.50    2.00    --  -48.00 -23.00 -16.30   50
 19  \w    -61.00 -34.00   0.50    2.00    --  -48.00 -23.00-116.03   54
 20  \w    -64.00 -35.00   0.50    2.00    --  -53.01 125.00 -60.00   58
 21  \w    -90.00 -37.00   0.50    2.00    --  -53.01   0.00 150.00  106
 22  \w    -88.00 -33.00   0.50    2.00    --  -53.01   0.00 -90.00  110
 23  \w    -87.00 -35.00   0.50    2.00    --  -53.01 -15.00  30.00  104
 24  \w    -70.00 -44.00   0.50    2.00    --  -60.00 -22.00  70.46   52
 25  \w    -70.00 -45.00   0.50    2.00    --  -60.00 -22.00  94.46   50
 26  \w    -70.00 -45.00   0.50    2.00    --  -60.50 -22.00-151.34   50
 27  \w    -71.00 -46.00   0.50    2.00    --  -60.50 -22.00-171.40   50
 28  \w    -70.00 -45.00   0.50    2.00    --  -60.50 -22.00 163.83   50
 29  \w    -71.00 -46.00   0.50    2.00    --  -60.50 -22.00-121.60   50
 30  \w     35.00  76.00   0.50    2.00    --   66.60-125.00-120.00   82
 31  \w     44.00  94.00   0.50    2.00    --   66.60-125.00 -30.00  100
 32  \w     35.00  92.00   0.50    2.00    --   66.60-125.00  90.00  114
 33  \w     67.00  95.00   0.50    2.00    --   66.60-125.00-180.00   56
 34  \w     35.00  63.00   0.50    2.00    --   66.60-125.00-180.00   56
 35  \w     29.00  54.00   0.50    2.00    --   66.60 -94.00 -90.00   50
 36  \w     36.00  97.00   0.50    2.00    --   69.84-125.00 120.00  122
 37  \w     79.00 107.00   0.50    2.00    --   69.84   0.00-120.00   56
 38  \w     36.00  76.00   0.50    2.00    --   69.84   0.00-120.00   80
 39  \w     50.00  91.00   0.50    2.00    --   69.84   0.00  90.00   82
 40  \w     36.00  96.00   0.50    2.00    --   69.84-125.00   0.00  120
 41  \w     39.00  92.00   0.50    2.00    --   69.84   0.00  30.00  106
 42  \w     38.00 103.00   0.50    2.00    --   72.00-130.00 -89.92  130
 43  \w     54.00  91.00   0.50    2.00    --   72.66  21.00-168.62   74
 44  \w     55.00  92.00   0.50    2.00    --   72.66  21.00  18.74   74
 45  \w     38.00 103.00   0.50    2.00    --   75.25-128.00  18.18  130
 46  \w     34.00  73.00   0.50    2.00    --   75.25-107.00 -71.55   78
 47  \w     32.00  65.00   0.50    2.00    --   75.25-116.00-157.89   66
 48  \w     40.00  65.00   0.50    2.00    --   75.25 -83.00 144.71   50
 49  \w     34.00 102.00   0.50    2.00    --   75.25-123.00-133.26  136
 50  \w     32.00 101.00   0.50    2.00    --   75.25-119.00  46.28  138
 51  \w     33.00  79.00   0.50    2.00    --   75.25-111.00  47.27   92
 52  \w     96.00 122.00   0.50    2.00    --   75.25  21.00 153.78   52
 53  \w     66.00  92.00   0.50    2.00    --   75.25  21.00 153.78   52
 54  \w     33.00  97.00   0.50    2.00    --   75.25-112.00  78.49  128
 55  \w     57.00 119.00   0.50    2.00    --   75.25  21.00 -93.33  124
 56  \w     76.00 104.00   0.50    2.00    --   75.25-126.00 143.58   56
 57  \w     37.00  72.00   0.50    2.00    --   75.25-126.00 143.58   70
 58  \w     51.00 109.00   0.50    2.00    --   75.25   1.00 126.19  116
 59  \w     34.00  98.00   0.50    2.00    --   75.25-114.00 151.47  128
 60  \w     71.00 103.00   0.50    2.00    --   75.25-123.00 -71.61   64
 61  \w     35.00  60.00   0.50    2.00    --   75.25-123.00 -71.61   50
 62  \w     59.00 113.00   0.50    2.00    --   75.25  21.00 -42.47  108
 63  \w     72.00  97.00   0.50    2.00    --   75.25-114.00  92.92   50
 64  \w     34.00  60.00   0.50    2.00    --   75.25-114.00  92.92   52
 65  \w     58.00  91.00   0.50    2.00    --   75.25  21.00 103.73   66
 66  \w     43.00  88.00   0.50    2.00    --   75.25   7.00 -29.39   90
 67  \w     41.00  86.00   0.50    2.00    --   75.25   4.00-167.46   90
 68  \w     71.00  98.00   0.50    2.00    --   75.25-114.00 -45.51   54
 69  \w     32.00  67.00   0.50    2.00    --   75.25-114.00 -45.51   70
 70  \w     83.00 116.00   0.50    2.00    --   75.25   4.00  17.06   66
 71  \w     42.00  80.00   0.50    2.00    --   75.25   4.00  17.06   76
 72  \w     69.00 102.00   0.50    2.00    --   75.25   3.00 -86.01   66
 73  \w     59.00 115.00   0.50    2.00    --   75.25  21.00  41.61  112
 74  \w     39.00  65.00   0.50    2.00    --   75.25   3.00 -86.01   52
 75  \w     57.00  95.00   0.50    2.00    --   75.25  20.00-132.01   76
 76  \w     91.00 116.00   0.50    2.00    --   75.25   4.00-167.46   50
 77  \w     69.00  95.00   0.50    2.00    --   75.25-116.00-157.89   52
 78  \w     62.00  87.00   0.50    2.00    --   75.25  21.00 132.66   50
 79  \w     59.00  95.00   0.50    2.00    --   75.25  21.00  73.47   72
;
_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      0.1389942000
_diffrn_orient_matrix_UB_12      -0.0682692000
_diffrn_orient_matrix_UB_13      -0.0026201000
_diffrn_orient_matrix_UB_21      0.0667855000
_diffrn_orient_matrix_UB_22      0.1312300000
_diffrn_orient_matrix_UB_23      -0.1012946000
_diffrn_orient_matrix_UB_31      0.0234627000
_diffrn_orient_matrix_UB_32      0.0506098000
_diffrn_orient_matrix_UB_33      0.0950019000
_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  0.0354
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            29393
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.872
_diffrn_reflns_theta_min         3.986
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.271
_exptl_absorpt_correction_T_max  0.778
_exptl_absorpt_correction_T_min  0.657
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.443
_exptl_crystal_description       block
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.139
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.025
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         4749
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0731P)^2^+0.3900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1164
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4508
_reflns_number_total             4749
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00126h2.cif
_cod_data_source_block           CrdpqCN
_cod_original_cell_volume        1202.71(5)
_cod_database_code               7709558
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C26 H21.53 Cr1 N6 O3.265'
_shelx_estimated_absorpt_t_max   0.726
_shelx_estimated_absorpt_t_min   0.588
_reflns_odcompleteness_completeness 98.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 1*[Sof(O4)+Sof(H4A)+Sof(H4B)]+1*[Sof(O6)+Sof(H6A)+Sof(H6B)]+1*[Sof(O5)+
 Sof(H5A)+Sof(H5B)]=1 with esd of 0.01
 Sof(O4)=Sof(H4A)=Sof(H4B)=FVAR(1)
 Sof(O6)=Sof(H6A)=Sof(H6B)=FVAR(2)
 Sof(O5)=Sof(H5A)=Sof(H5B)=FVAR(3)
 Sof(O1)=Sof(H1A)=Sof(H1B)=FVAR(4)
 Sof(O3)=Sof(H3A)=Sof(H3B)=FVAR(5)
3.a Riding coordinates:
 O2(H2A,H2B)
3.b Free rotating group:
 O1(H1A,H1B), O3(H3A,H3B), O4(H4A,H4B), O5(H5A,H5B), O6(H6A,H6B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15),
 C16(H16), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25), C26(H26)
;
_shelx_res_checksum              85488
_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 1.900
_oxdiff_exptl_absorpt_empirical_full_min 0.747