Chiral Molecular Ruby [Cr(dqp)<sub>2</sub>]<sup>3+</sup> with Long-Lived Circularly Polarized Luminescence.
Jiménez, Juan-Ramón; Doistau, Benjamin; Cruz, Carlos M.; Besnard, Céline; Cuerva, Juan M.; Campaña, Araceli G; Piguet, Claude; Journal of the American Chemical Society 141 (2019) 13244–13252; doi:10.1021/jacs.9b06524

data_4127843
_publ_section_title
;
 Chiral Molecular Ruby [Cr(dqp)<sub>2</sub>]<sup>3+</sup> with Long-Lived
 Circularly Polarized Luminescence.
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13244
_journal_page_last               13252
_journal_paper_doi               10.1021/jacs.9b06524
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C46 H30 Cr N6, 3(C F3 O3 S), C2 H3 N'
_chemical_formula_sum            'C51 H33 Cr F9 N7 O9 S3'
_chemical_formula_weight         1207.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2019-02-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                86.510(3)
_cell_angle_beta                 80.088(3)
_cell_angle_gamma                84.768(3)
_cell_formula_units_Z            2
_cell_length_a                   11.1216(4)
_cell_length_b                   13.1420(4)
_cell_length_c                   17.3331(7)
_cell_measurement_reflns_used    11409
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      70.8660
_cell_measurement_theta_min      4.3480
_cell_volume                     2482.56(16)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      180.15
_diffrn_detector_area_resol_mean 10.4670
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9762
_diffrn_measured_fraction_theta_max 0.9762
_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    -72.00  22.00   1.00    1.01    --  -42.25  77.00 -90.00   94
  2  \w   -112.00 -16.00   1.00    1.01    --  -42.25 -57.00   0.00   96
  3  \w    -63.00  26.00   1.00    1.01    --  -42.25  57.00 150.00   89
  4  \w     53.00  80.00   1.00    5.00    --  100.00 -61.00-180.00   27
  5  \w     31.00 128.00   1.00    5.00    --  100.00 -61.00 -90.00   97
  6  \w    128.00 161.00   1.00    5.00    --  100.00  77.00  60.00   33
  7  \w     76.00 170.00   1.00    5.00    --  100.00  45.00-120.00   94
  8  \w     90.00 158.00   1.00    5.00    --  100.00  45.00   0.00   68
  9  \w     29.00  62.00   1.00    5.00    --  100.00-125.00   0.00   33
 10  \w     81.00 113.00   1.00    5.00    --  100.00-125.00   0.00   32
 11  \w    104.00 172.00   1.00    5.00    --  100.00 125.00-120.00   68
 12  \w     38.00 114.00   1.00    5.00    --  100.00-125.00  90.00   76
 13  \w     33.00 118.00   1.00    5.00    --  100.00-125.00-150.00   85
 14  \w     99.00 133.00   1.00    5.00    --  100.00 125.00-180.00   34
 15  \w     38.00  92.00   1.00    5.00    --  100.00-125.00-120.00   54
 16  \w     52.00  81.00   1.00    5.00    --  100.00 -61.00  30.00   29
 17  \w     99.00 124.00   1.00    5.00    --  100.00 -61.00  30.00   25
 18  \w     44.00 101.00   1.00    5.00    --  100.00-125.00 -60.00   57
 19  \w     77.00 155.00   1.00    5.00    --  100.00  30.00 150.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19596
_diffrn_reflns_theta_full        70.8972
_diffrn_reflns_theta_max         70.90
_diffrn_reflns_theta_min         4.05
_exptl_absorpt_coefficient_mu    3.967
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.358
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.6146
_exptl_crystal_description       plate
_exptl_crystal_F_000             1232.2572
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.247
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.4004
_refine_diff_density_min         -0.4088
_refine_diff_density_rms         0.0568
_refine_ls_d_res_high            0.8158
_refine_ls_d_res_low             10.9186
_refine_ls_goodness_of_fit_ref   1.0434
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    64
_refine_ls_number_parameters     722
_refine_ls_number_reflns         9343
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0434
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.0058
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+0.8483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.0962
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                8814
_reflns_number_total             9343
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja9b06524_si_001.cif
_cod_data_source_block           jr193t
_cod_original_cell_volume        2482.55(15)
_cod_database_code               4127843
_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:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13),
 C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
  C26(H26), C28(H28), C29(H29), C30(H30), C34(H34), C35(H35), C36(H36),
 C39(H39), C40(H40), C41(H41), C44(H44), C45(H45), C46(H46)
2.b Idealised Me refined as rotating group:
 C53(H53a,H53b,H53c)
;
_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
;