Luminescent polypyridyl heteroleptic Cr<sup>III</sup> complexes with high quantum yields and long excited state lifetimes.
Jiménez, Juan-Ramón; Poncet, Maxime; Doistau, Benjamin; Besnard, Céline; Piguet, Claude; Dalton transactions (Cambridge, England : 2003) 49 (2020) 13528–13532; doi:10.1039/d0dt02872j

data_7705367
_publ_section_title
;
 Luminescent polypyridyl heteroleptic Cr<sup>III</sup> complexes with high
 quantum yields and long excited state lifetimes.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13528
_journal_page_last               13532
_journal_paper_doi               10.1039/d0dt02872j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C40 H32 Cr N8, 3(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C44 H38 Cr F18 N10 P3'
_chemical_formula_weight         1193.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-07-09 deposited with the CCDC.	2020-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.3997(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.14124(15)
_cell_length_b                   22.83951(17)
_cell_length_c                   20.55852(15)
_cell_measurement_reflns_used    40372
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      70.8600
_cell_measurement_theta_min      2.1240
_cell_volume                     9926.55(13)
_computing_cell_refinement       'CrysAlisPro 1.171.41.53a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.53a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.53a (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      149.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-Arc
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.943
_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    -69.00 -39.00   0.50    6.00    --  -52.43 -15.00-180.00   60
  2  \w    -72.00 -17.00   0.50    6.00    --  -52.43 125.00 -90.00  110
  3  \w    -82.00 -25.00   0.50    6.00    --  -52.43 -15.00  60.00  114
  4  \w    -90.00 -24.00   0.50    6.00    --  -52.43 -15.00 -60.00  132
  5  \w    -71.00 -28.00   0.50    6.00    --  -60.50 124.00 160.34   86
  6  \w   -101.00 -76.00   0.50    6.00    --  -60.50 -52.00 173.88   50
  7  \w    -51.00 -26.00   0.50    6.00    --  -60.50 136.00 -31.91   50
  8  \w    -81.00 -53.00   0.50    6.00    --  -60.50 136.00 -31.91   56
  9  \w     86.00 111.00   0.50    6.00    --   68.74  15.00-120.00   50
 10  \w     35.00  67.00   0.50    6.00    --   68.74-125.00-120.00   64
 11  \w     41.00  92.00   0.50    6.00    --   68.74-125.00 120.00  102
 12  \w     41.00  77.00   0.50    6.00    --   68.74  15.00-120.00   72
 13  \w     61.00  95.00   0.50    6.00    --   68.74  15.00-180.00   68
 14  \w     34.00  94.00   0.50    6.00    --   68.74-125.00 -90.00  120
 15  \w     36.00  68.00   0.50    6.00    --   68.74-125.00 -60.00   64
 16  \w     40.00 102.00   0.50    6.00    --   68.74  15.00 -30.00  124
 17  \w     46.00  79.00   0.50    6.00    --   68.74  15.00  60.00   66
 18  \w     51.00  77.00   0.50    6.00    --   68.74-125.00  60.00   52
 19  \w     80.00 105.00   0.50    6.00    --   68.74  15.00 150.00   50
 20  \w     41.00  70.00   0.50    6.00    --   68.74  15.00 150.00   58
 21  \w     49.00  90.00   0.50    6.00    --   68.74-125.00-150.00   82
 22  \w     65.00  93.00   0.50    6.00    --   68.74  15.00-150.00   56
 23  \w     40.00  92.00   0.50    6.00    --   68.74-125.00  30.00  104
 24  \w     48.00  96.00   0.50    6.00    --   68.74  15.00  90.00   96
 25  \w     36.00  61.00   0.50    6.00    --   68.74-125.00 -30.00   50
 26  \w     54.00 108.00   0.50    6.00    --   74.34  18.00 120.98  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0091250273
_diffrn_orient_matrix_UB_12      -0.0388124701
_diffrn_orient_matrix_UB_13      -0.0606408314
_diffrn_orient_matrix_UB_21      0.0704571917
_diffrn_orient_matrix_UB_22      -0.0170902512
_diffrn_orient_matrix_UB_23      0.0027920997
_diffrn_orient_matrix_UB_31      -0.0161802113
_diffrn_orient_matrix_UB_32      -0.0524511865
_diffrn_orient_matrix_UB_33      0.0439512112
_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  0.0541
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            87579
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.785
_diffrn_reflns_theta_min         2.090
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.837
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.53a (Rigaku Oxford Diffraction, 2020)
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    1.598
_exptl_crystal_description       plate
_exptl_crystal_F_000             4824
_exptl_crystal_size_max          0.637
_exptl_crystal_size_mid          0.394
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1377
_refine_ls_number_reflns         18950
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0880P)^2^+7.3983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1505
_refine_ls_wR_factor_ref         0.1579
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15427
_reflns_number_total             18950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02872j2.cif
_cod_data_source_block           jr286_2
_cod_depositor_comments
'Adding full bibliography for 7705367--7705370.cif.'
_cod_original_cell_volume        9926.55(12)
_cod_database_code               7705367
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C44 H38 Cr1 F18 N10 P3'
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.194
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H7SA,H7SB,H7SC} of C7S
 At 1.5 times of:
  {H29A,H29B,H29C} of C29, {H35A,H35B,H35C} of C35, {H35D,H35E,H35F} of C35B,
  {H29D,H29E,H29F} of C29B, {H6SA,H6SB,H6SC} of C6S, {H12A,H12C,H12D} of C12S,
  {H1SA,H1SB,H1SC} of C1S
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13),
 C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25),
  C26(H26), C27(H27), C31(H31), C32(H32), C33(H33), C37(H37), C38(H38),
 C39(H39), C40(H40), C23B(H23B), C22B(H22B), C21B(H21B), C18B(H18B), C17B(H17B),
  C16B(H16B), C13B(H13B), C12B(H12B), C11B(H11B), C8B(H8B), C7B(H7B), C6B(H6B),
 C3B(H3B), C2B(H2B), C1B(H1B), C24B(H24B), C25B(H25B), C26B(H26B), C27B(H27B),
 C31B(H31B), C32B(H32B), C33B(H33B), C37B(H37B), C38B(H38B), C39B(H39B),
 C40B(H40B)
2.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C35(H35A,H35B,H35C), C29B(H29D,H29E,H29F), C35B(H35D,
 H35E,H35F), C1S(H1SA,H1SB,H1SC), C6S(H6SA,H6SB,H6SC), C7S(H7SA,H7SB,H7SC),
 C12S(H12A,H12C,H12D)
;
_shelx_res_checksum              850
_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 5.489
_oxdiff_exptl_absorpt_empirical_full_min 0.308