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_7705370
_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
'C38 H26 Cr N6, 2.826(F6 P), 0.174(C F3 O3 S), 2(C2 H3 N)'
_chemical_formula_sum            'C42.17 H32 Cr F17.48 N8 O0.52 P2.83 S0.17'
_chemical_formula_weight         1136.37
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-10
_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
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.10349(6)
_cell_length_b                   17.98863(8)
_cell_length_c                   28.79512(12)
_cell_measurement_reflns_used    64902
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      74.1070
_cell_measurement_theta_min      2.4620
_cell_volume                     8859.35(6)
_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 1.000
_diffrn_measured_fraction_theta_max 0.994
_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    -57.00 -26.00   0.50    1.50    --  -52.43 125.00-180.00   62
  2  \w    -80.00 -44.00   0.50    1.50    --  -52.43   0.00  30.00   72
  3  \w    -73.00 -13.00   0.50    1.50    --  -52.43 125.00 -60.00  120
  4  \w     42.00 100.00   0.50    1.50    --   69.83   0.00 -30.00  116
  5  \w     42.00 104.00   0.50    1.50    --   69.83  15.00   0.00  124
  6  \w     46.00  92.00   0.50    1.50    --   69.83  15.00  60.00   92
  7  \w     34.00  59.00   0.50    1.50    --   72.00-106.00  32.74   50
  8  \w     65.00  90.00   0.50    1.50    --   75.25  22.00-126.69   50
  9  \w     41.00  82.00   0.50    1.50    --   75.25 -97.00 -11.91   82
 10  \w     43.00  69.00   0.50    1.50    --   75.25-129.00  53.92   52
 11  \w     51.00  77.00   0.50    1.50    --   75.25-101.00 162.48   52
 12  \w     52.00  77.00   0.50    1.50    --   75.25 -94.00  46.80   50
 13  \w     38.00  78.00   0.50    1.50    --   75.25-103.00 -15.60   80
 14  \w     60.00 105.00   0.50    1.50    --   75.25   1.00  88.32   90
 15  \w     41.00  82.00   0.50    1.50    --   75.25-102.00-140.87   82
 16  \w     38.00  83.00   0.50    1.50    --   75.25-104.00-112.59   90
 17  \w     43.00  69.00   0.50    1.50    --   75.25 -77.00 -12.91   52
 18  \w     44.00  69.00   0.50    1.50    --   75.25 -81.00  99.73   50
 19  \w     85.00 110.00   0.50    1.50    --   75.25   1.00  30.78   50
 20  \w     62.00  88.00   0.50    1.50    --   75.25   7.00-103.59   52
 21  \w     67.00 110.00   0.50    1.50    --   75.25   1.00-126.55   86
 22  \w     84.00 115.00   0.50    1.50    --   75.25  16.00 121.81   62
 23  \w     73.00  98.00   0.50    1.50    --   75.25  21.00 147.93   50
 24  \w     65.00 111.00   0.50    1.50    --   75.25  17.00  33.46   92
 25  \w     35.00  60.00   0.50    1.50    --   75.25 -53.00 107.38   50
 26  \w     51.00  87.00   0.50    1.50    --   75.25   3.00 -42.47   72
 27  \w     43.00  68.00   0.50    1.50    --   75.25   4.00-162.90   50
 28  \w     42.00  84.00   0.50    1.50    --   75.25-102.00  49.93   84
 29  \w     45.00  70.00   0.50    1.50    --   75.25 -96.00 -94.06   50
 30  \w     40.00  69.00   0.50    1.50    --   75.25-107.00 102.03   58
 31  \w     45.00  78.00   0.50    1.50    --   75.25 -94.00  28.78   66
 32  \w     69.00  94.00   0.50    1.50    --   75.25  22.00  -0.51   50
 33  \w     34.00  71.00   0.50    1.50    --   75.25-122.00 -55.65   74
 34  \w     39.00  64.00   0.50    1.50    --   75.25-100.00  81.32   50
 35  \w     41.00  66.00   0.50    1.50    --   75.25 -73.00-158.29   50
 36  \w     89.00 109.00   0.50    1.50    --   75.25  22.00  69.71   40
;
_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      -0.0432670000
_diffrn_orient_matrix_UB_12      0.0404730000
_diffrn_orient_matrix_UB_13      -0.0395447000
_diffrn_orient_matrix_UB_21      0.0187605000
_diffrn_orient_matrix_UB_22      -0.0648535000
_diffrn_orient_matrix_UB_23      -0.0331222000
_diffrn_orient_matrix_UB_31      -0.0767267000
_diffrn_orient_matrix_UB_32      -0.0386442000
_diffrn_orient_matrix_UB_33      0.0141787000
_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  0.0245
_diffrn_reflns_av_unetI/netI     0.0096
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            95378
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.427
_diffrn_reflns_theta_min         3.069
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.261
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.180
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.53a (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    1.704
_exptl_crystal_description       block
_exptl_crystal_F_000             4574
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.243
_exptl_crystal_size_min          0.189
_refine_diff_density_max         1.594
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         8997
_refine_ls_number_restraints     137
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0594P)^2^+12.0072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1206
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8817
_reflns_number_total             8997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02872j2.cif
_cod_data_source_block           jr272
_cod_depositor_comments
'Adding full bibliography for 7705367--7705370.cif.'
_cod_database_code               7705370
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula
'C42.175 H32 Cr1 F17.474 N8 O0.526 P2.825 S0.175'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.46
_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. Restrained distances
 S1-O1 \\sim S1-O2 \\sim S1-O3
 with sigma of 0.02
 F19-C41 \\sim F20-C41 \\sim F21-C41
 with sigma of 0.02
 P3-F16 \\sim P3-F14 \\sim P3-F15 \\sim P3-F18 \\sim P3-F17 \\sim P3-F13
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F14) = Uanis(O2)
Uanis(F13) = Uanis(O1)
4. Rigid body (RIGU) restrains
 F17, P3, F13, F15, F18, F14, F16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, O2, S1, C41, O1, F19, F20, F21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O2)=Sof(F19)=Sof(S1)=Sof(C41)=Sof(F20)=Sof(F21)=Sof(O3)=Sof(O1)=1-FVAR(1)
 Sof(P3)=Sof(F13)=Sof(F15)=Sof(F18)=Sof(F17)=Sof(F14)=Sof(F16)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C8(H8), C24(H24), C6(H6), C2(H2), C12(H12), C11(H11), C37(H37),
 C38(H38), C7(H7), C13(H13), C3(H3), C16(H16), C17(H17), C23(H23), C35(H35),
 C36(H36), C18(H18), C25(H25), C32(H32), C30(H30), C27(H27), C31(H31), C26(H26),
  C22(H22), C21(H21)
6.b Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              4142
_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 1.113
_oxdiff_exptl_absorpt_empirical_full_min 0.872