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_7709557
_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         'C20 H17 Cr N8, 2(H2 O)'
_chemical_formula_sum            'C20 H21 Cr N8 O2'
_chemical_formula_weight         457.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-29
_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                90
_cell_angle_beta                 102.2381(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9309(2)
_cell_length_b                   13.5078(2)
_cell_length_c                   13.8221(3)
_cell_measurement_reflns_used    15089
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.0430
_cell_measurement_theta_min      4.9870
_cell_volume                     2176.95(7)
_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(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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    -87.00 -57.00   0.50    0.50    --  -53.01 -15.00-150.00   60
  2  \w    -53.00 -25.00   0.50    0.50    --  -53.01 -15.00-150.00   56
  3  \w    -67.00 -41.00   0.50    0.50    --  -53.01 125.00 120.00   52
  4  \w     44.00  99.00   0.50    0.50    --   66.60  15.00 120.00  110
  5  \w     37.00  64.00   0.50    0.50    --   66.60-125.00  60.00   54
  6  \w     69.00  95.00   0.50    0.50    --   66.60-125.00  60.00   52
  7  \w     59.00 112.00   0.50    0.50    --   66.60  15.00  30.00  106
  8  \w     31.00  71.00   0.50    0.50    --   66.60 -94.00-120.00   80
  9  \w     71.00  98.00   0.50    0.50    --   69.84-125.00   0.00   54
 10  \w     37.00  75.00   0.50    0.50    --   69.84 -94.00-150.00   76
 11  \w     35.00  78.00   0.50    0.50    --   69.84 -94.00  60.00   86
 12  \w     41.00  78.00   0.50    0.50    --   69.84  15.00-180.00   74
 13  \w     80.00 106.00   0.50    0.50    --   69.84  15.00-180.00   52
 14  \w     33.00  61.00   0.50    0.50    --   75.25 -55.00  96.40   56
 15  \w     32.00  57.00   0.50    0.50    --   75.25 -53.00 -61.17   50
 16  \w     48.00  90.00   0.50    0.50    --   75.25  19.00 -79.90   84
 17  \w     45.00  91.00   0.50    0.50    --   75.25  12.00-117.57   92
 18  \w     40.00  70.00   0.50    0.50    --   75.25 -73.00 168.40   60
 19  \w     53.00  99.00   0.50    0.50    --   75.25-127.00-159.35   92
 20  \w     41.00  66.00   0.50    0.50    --   75.25-105.00 122.06   50
 21  \w     48.00 118.00   0.50    0.50    --   75.25  15.00   6.14  140
 22  \w     69.00  94.00   0.50    0.50    --   75.25-113.00 -68.98   50
 23  \w     36.00  62.00   0.50    0.50    --   75.25 -62.00 145.56   52
 24  \w     78.00 113.00   0.50    0.50    --   75.25   4.00 168.38   70
 25  \w     46.00  72.00   0.50    0.50    --   75.25   4.00 168.38   52
 26  \w     57.00 118.00   0.50    0.50    --   75.25  14.00  67.42  122
 27  \w     63.00  89.00   0.50    0.50    --   75.25   2.00 -55.46   52
 28  \w     36.00  61.00   0.50    0.50    --   75.25-113.00 -68.98   50
 29  \w     47.00  86.00   0.50    0.50    --   75.25-101.00-126.02   78
 30  \w     74.00 104.00   0.50    0.50    --   75.25-132.00 158.32   60
 31  \w     33.00  58.00   0.50    0.50    --   75.25 -52.00 -24.14   50
 32  \w    -87.00 -60.00   0.50    0.50    --  -53.01   0.00 -60.00   54
 33  \w    -49.00 -16.00   0.50    0.50    --  -53.01   0.00 -60.00   66
 34  \w    -68.00 -42.00   0.50    0.50    --  -53.01 125.00-150.00   52
 35  \w    -53.00 -20.00   0.50    0.50    --  -53.01   0.00-150.00   66
 36  \w    -67.00 -39.00   0.50    0.50    --  -53.01 125.00  60.00   56
 37  \w    -80.00 -54.00   0.50    0.50    --  -53.01   0.00-150.00   52
 38  \w     59.00  85.00   0.50    0.50    --   66.60-125.00-120.00   52
 39  \w     29.00  54.00   0.50    0.50    --   66.60 -94.00  60.00   50
 40  \w     47.00  73.00   0.50    0.50    --   66.60 -94.00 120.00   52
 41  \w     31.00  73.00   0.50    0.50    --   66.60 -94.00 -60.00   84
 42  \w     70.00  95.00   0.50    0.50    --   66.60-125.00 -90.00   50
 43  \w     85.00 115.00   0.50    0.50    --   69.84  15.00-120.00   60
 44  \w     73.00  98.00   0.50    0.50    --   69.84-125.00-180.00   50
 45  \w     45.00  79.00   0.50    0.50    --   69.84  15.00-120.00   68
 46  \w     73.00  98.00   0.50    0.50    --   69.84-125.00 -90.00   50
 47  \w     44.00  97.00   0.50    0.50    --   69.84  15.00 -30.00  106
 48  \w     40.00  75.00   0.50    0.50    --   75.25 -87.00  58.61   70
 49  \w     40.00  67.00   0.50    0.50    --   75.25 -77.00  -6.35   54
 50  \w     39.00  64.00   0.50    0.50    --   75.25 -89.00-111.49   50
 51  \w     37.00  63.00   0.50    0.50    --   75.25 -60.00   7.64   52
 52  \w     48.00  96.00   0.50    0.50    --   75.25-111.00 -31.70   96
 53  \w     63.00 102.00   0.50    0.50    --   75.25-121.00 -64.35   78
 54  \w     43.00  73.00   0.50    0.50    --   75.25 -84.00 -62.61   60
 55  \w     73.00  98.00   0.50    0.50    --   75.25-114.00 -52.69   50
 56  \w     54.00 102.00   0.50    0.50    --   75.25-121.00  22.33   96
 57  \w     98.00 123.00   0.50    0.50    --   75.25-155.00 128.92   50
 58  \w     64.00  90.00   0.50    0.50    --   75.25-155.00 128.92   52
 59  \w     65.00  90.00   0.50    0.50    --   75.25-111.00  19.16   50
 60  \w     60.00  86.00   0.50    0.50    --   75.25 -98.00-159.00   52
 61  \w     77.00 113.00   0.50    0.50    --   75.25  19.00 143.22   72
 62  \w     48.00  74.00   0.50    0.50    --   75.25-103.00 -66.48   52
 63  \w     52.00  78.00   0.50    0.50    --   75.25  19.00-126.16   52
 64  \w     60.00 103.00   0.50    0.50    --   75.25-123.00 128.99   86
 65  \w     87.00 112.00   0.50    0.50    --   75.25-140.00-105.30   50
 66  \w     46.00  72.00   0.50    0.50    --   75.25   1.00  -2.78   52
 67  \w     66.00  96.00   0.50    0.50    --   75.25-112.00  55.04   60
;
_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      -0.0983626000
_diffrn_orient_matrix_UB_12      -0.0547298000
_diffrn_orient_matrix_UB_13      0.0335219000
_diffrn_orient_matrix_UB_21      0.0642909000
_diffrn_orient_matrix_UB_22      0.0094022000
_diffrn_orient_matrix_UB_23      0.1087159000
_diffrn_orient_matrix_UB_31      -0.0603891000
_diffrn_orient_matrix_UB_32      0.0996255000
_diffrn_orient_matrix_UB_33      0.0081480000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0109
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20649
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.389
_diffrn_reflns_theta_min         5.011
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.613
_exptl_absorpt_correction_T_max  0.448
_exptl_absorpt_correction_T_min  0.178
_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    1.396
_exptl_crystal_description       block
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.848
_exptl_crystal_size_mid          0.358
_exptl_crystal_size_min          0.238
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2182
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0257
_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^)+(0.0408P)^2^+1.3549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0740
_refine_ls_wR_factor_ref         0.0741
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2160
_reflns_number_total             2182
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00126h2.cif
_cod_data_source_block           CrddpdCN
_cod_original_cell_volume        2176.94(7)
_cod_database_code               7709557
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H21 Cr1 N8 O2'
_shelx_estimated_absorpt_t_max   0.407
_shelx_estimated_absorpt_t_min   0.111
_reflns_odcompleteness_completeness 99.91
_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 C(H,H,H) groups, All O(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_shelx_res_checksum              17924
_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 1.421
_oxdiff_exptl_absorpt_empirical_full_min 0.551