Versatile heteroleptic bis-terdentate Cr(iii) chromophores displaying room temperature millisecond excited state lifetimes.
Jiménez, Juan-Ramón; Doistau, Benjamin; Besnard, Céline; Piguet, Claude; Chemical communications (Cambridge, England) 54 (2018) 13228–13231; doi:10.1039/c8cc07671e

data_7122545
_publ_section_title
;
 Versatile heteroleptic bis-terdentate Cr(iii) chromophores displaying
 room temperature millisecond excited state lifetimes.
;
_journal_issue                   94
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13228
_journal_page_last               13231
_journal_paper_doi               10.1039/c8cc07671e
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C17 H17 Br3 Cr N5'
_chemical_formula_sum            'C17 H17 Br3 Cr N5'
_chemical_formula_weight         583.08
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-20 deposited with the CCDC.
2018-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.8596(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.35425(14)
_cell_length_b                   15.1963(2)
_cell_length_c                   13.72684(18)
_cell_measurement_reflns_used    9255
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      70.4460
_cell_measurement_theta_min      4.3270
_cell_volume                     1941.07(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4670
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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   -116.00 -27.00   1.00    1.00    --  -41.64 -38.00   0.00   89
  2  \w    -92.00 -34.00   1.00    1.00    --  -41.64 125.00 -60.00   58
  3  \w    -27.00  -2.00   1.00    1.00    --  -41.64 125.00 -60.00   25
  4  \w      1.00  27.00   1.00    1.00    --   41.64 -99.00 -60.00   26
  5  \w     98.00 140.00   1.00    1.65    --  100.00 125.00-120.00   42
  6  \w    113.00 167.00   1.00    3.21    --  100.00 125.00-150.00   54
  7  \w     29.00 126.00   1.00    3.21    --  100.00 -61.00-180.00   97
  8  \w     36.00 107.00   1.00    3.21    --  100.00-125.00-180.00   71
  9  \w     71.00 161.00   1.00    3.21    --  100.00  61.00 -30.00   90
 10  \w     73.00 174.00   1.00    3.21    --  100.00  30.00  60.00  101
 11  \w      0.00  26.00   1.00    1.00    --  -41.74   0.00-150.00   26
 12  \w    -68.00 -28.00   1.00    1.00    --  -41.74 -57.00  30.00   40
 13  \w    -41.00 -15.00   1.00    1.00    --  -41.74   0.00-150.00   26
 14  \w    -93.00 -30.00   1.00    1.00    --  -41.74 -38.00  60.00   63
 15  \w   -124.00 -69.00   1.00    1.00    --  -41.74   0.00-150.00   55
 16  \w     39.00 115.00   1.00    3.21    --  100.00-125.00-150.00   76
 17  \w     67.00  92.00   1.00    3.21    --  100.00  77.00  30.00   25
 18  \w     71.00 152.00   1.00    3.21    --  100.00  61.00  90.00   81
 19  \w     84.00 110.00   1.00    3.21    --  100.00-125.00 -60.00   26
 20  \w    147.00 172.00   1.00    3.21    --  100.00  61.00  60.00   25
 21  \w    150.00 175.00   1.00    3.21    --  100.00  77.00  90.00   25
 22  \w     73.00  99.00   1.00    3.21    --  100.00  61.00  60.00   26
 23  \w    148.00 173.00   1.00    3.21    --  100.00  77.00  30.00   25
 24  \w     67.00  93.00   1.00    3.21    --  100.00  77.00  60.00   26
 25  \w    145.00 171.00   1.00    3.21    --  100.00  61.00 120.00   26
 26  \w     82.00 134.00   1.00    3.21    --  100.00  61.00 120.00   52
 27  \w    131.00 171.00   1.00    3.21    --  100.00  45.00 -90.00   40
 28  \w     74.00 100.00   1.00    3.21    --  100.00  45.00  90.00   26
 29  \w    122.00 172.00   1.00    3.21    --  100.00  77.00   0.00   50
 30  \w     71.00  96.00   1.00    3.21    --  100.00  61.00  30.00   25
 31  \w     68.00  93.00   1.00    3.21    --  100.00  77.00  90.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0751800000
_diffrn_orient_matrix_UB_12      -0.0127524000
_diffrn_orient_matrix_UB_13      -0.0938271000
_diffrn_orient_matrix_UB_21      0.1190279000
_diffrn_orient_matrix_UB_22      -0.0540061000
_diffrn_orient_matrix_UB_23      0.0583718000
_diffrn_orient_matrix_UB_31      -0.0870509000
_diffrn_orient_matrix_UB_32      -0.0848049000
_diffrn_orient_matrix_UB_33      -0.0229945000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17654
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.471
_diffrn_reflns_theta_min         4.353
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.180
_exptl_absorpt_correction_T_max  0.538
_exptl_absorpt_correction_T_min  0.154
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            'dark green'
_exptl_crystal_density_diffrn    1.995
_exptl_crystal_description       block
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.218
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.368
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0367
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1247
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3393
_reflns_number_total             3696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07671e2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7122544--7122546.cif.'
_cod_original_cell_volume        1941.08(5)
_cod_database_code               7122545
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C17 H17 Br3 Cr1 N5'
_shelx_estimated_absorpt_t_max   0.262
_shelx_estimated_absorpt_t_min   0.139
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C13(H13), C14(H14), C15(H15), C19(H19),
 C20(H20), C21(H21), C22(H22)
2.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              70912
_shelx_hkl_checksum              17570
_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 1.920
_oxdiff_exptl_absorpt_empirical_full_min 0.541