Circularly polarized near-infrared phosphorescence of chiral chromium(III) complexes.
Cheng, Yang; He, Jiang; Zou, Wenjie; Chang, Xiaoyong; Yang, Qingqing; Lu, Wei; Chemical communications (Cambridge, England) 59 (2023) 1781–1784; doi:10.1039/d2cc06548g

data_7131191
_publ_section_title
;
 Circularly polarized near-infrared phosphorescence of chiral
 chromium(III) complexes.
;
_journal_issue                   13
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1781
_journal_page_last               1784
_journal_paper_doi               10.1039/d2cc06548g
_journal_volume                  59
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C56 H68 Cr N6 O4, 2(C H2 Cl2), F6 P'
_chemical_formula_sum            'C58 H72 Cl4 Cr F6 N6 O4 P'
_chemical_formula_weight         1255.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2dmdk0
_audit_creation_date             2022-02-18
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-11-30 deposited with the CCDC.	2023-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.9030(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.2991(5)
_cell_length_b                   19.7818(8)
_cell_length_c                   12.9910(5)
_cell_measurement_reflns_used    9032
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.27
_cell_volume                     3039.7(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker PHOTON 100 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker CMOS area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            66954
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.592
_diffrn_reflns_theta_min         2.268
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.459
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0860 before and 0.0570 after correction.
The Ratio of minimum to maximum transmission is 0.9436.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       block
_exptl_crystal_F_000             1310
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 6775 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     747
_refine_ls_number_reflns         18667
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0442P)^2^+0.9814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0957
_reflns_Friedel_coverage         0.947
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                15963
_reflns_number_total             18667
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06548g2.cif
_cod_data_source_block           cxy1887_0m
_cod_depositor_comments
'Adding full bibliography for 7131190--7131192.cif.'
_cod_database_code               7131191
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.838
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl4A-C58A = Cl4-C58 = Cl3A-C58A = Cl3-C58
 1.79 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl4) = Uanis(Cl4A)
Uanis(C58) = Uanis(C58A)
Uanis(Cl3) = Uanis(Cl3A)
4. Others
 Sof(Cl3A)=Sof(Cl4A)=Sof(C58A)=Sof(H58C)=Sof(H58D)=1-FVAR(1)
 Sof(Cl3)=Sof(Cl4)=Sof(C58)=Sof(H58A)=Sof(H58B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C26(H26), C29(H29), C46(H46)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C27(H27A,H27B), C31(H31A,H31B), C47(H47A,H47B), C57(H57A,H57B),
 C58(H58A,H58B), C58A(H58C,H58D)
5.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12), C17(H17), C23(H23), C37(H37), C43(H43), C50(H50), C56(H56)
5.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C28(H28A,
 H28B,H28C), C30(H30A,H30B,H30C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C48(H48A,H48B,H48C), C53(H53A,H53B,H53C), C54(H54A,H54B,
 H54C), C55(H55A,H55B,H55C)
;
_shelx_res_checksum              24644
_shelx_hkl_checksum              1975
_olex2_submission_special_instructions 'No special instructions were received'