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_7131192
_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_formula_moiety         'C52 H60 Cr N6 O4, C H2 Cl2, 2(F3 P0.5)'
_chemical_formula_sum            'C53 H62 Cl2 Cr F6 N6 O4 P'
_chemical_formula_weight         1114.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2dmdn3
_audit_creation_date             2023-01-09
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-01-12 deposited with the CCDC.	2023-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.666(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.3793(15)
_cell_length_b                   19.1458(10)
_cell_length_c                   21.6094(11)
_cell_measurement_reflns_used    9107
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      68.13
_cell_measurement_theta_min      3.20
_cell_volume                     10294.0(10)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Apex3 (Bruker 2018)'
_computing_data_reduction        'SAINT V8.40B (?, 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 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2014'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Bruker PHOTON II area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            75165
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.378
_diffrn_reflns_theta_min         2.912
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    3.708
_exptl_absorpt_correction_T_max  0.1665
_exptl_absorpt_correction_T_min  0.0480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1364 before and 0.0777 after correction.
The Ratio of minimum to maximum transmission is 0.2883.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       block
_exptl_crystal_F_000             4648
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         9400
_refine_ls_number_restraints     167
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+23.5005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1340
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8247
_reflns_number_total             9400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06548g2.cif
_cod_data_source_block           cxy3440_2_0m
_cod_depositor_comments
'Adding full bibliography for 7131190--7131192.cif.'
_cod_database_code               7131192
_shelx_shelxl_version_number     2019/2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P1-F7
 1.62 with sigma of 0.02
 Cl2A-C53A = Cl1A-C53A = Cl1-C53 = Cl2-C53
 1.79 with sigma of 0.02
 F8-F7
 2.28 with sigma of 0.04
 Cl2A-Cl1A = Cl1-Cl2
 2.9 with sigma of 0.04
 P2-F5 \\sim P2-F5A \\sim P2-F4 \\sim P2-F6A \\sim P2-F4A \\sim P2-F6
 with sigma of 0.02
 P1-F2 \\sim P1-F3A \\sim P1-F2A \\sim P1-F1 \\sim P1-F3
 with sigma of 0.02
 O4A-C34 \\sim O4-C34
 with sigma of 0.02
 O4A-C35 \\sim O4-C35
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
P1 \\sim F1 \\sim F2 \\sim F2A \\sim F3 \\sim F3A \\sim F7 \\sim F8: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
P2 \\sim F4 \\sim F4A \\sim F5 \\sim F5A \\sim F6 \\sim F6A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(F3) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F2A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F4) = Uanis(F4A)
Uanis(F6) = Uanis(F6A)
Uanis(F5) = Uanis(F5A)
Uanis(O4) = Uanis(O4A)
Uanis(Cl2) = Uanis(Cl2A)
Uanis(C53) = Uanis(C53A)
Uanis(Cl1) = Uanis(Cl1A)
4. Others
 Sof(F7)=Sof(F8)=1-FVAR(1)
 Sof(F2)=Sof(F2A)=Sof(F3)=Sof(F3A)=0.5*FVAR(2)
 Sof(Cl2A)=Sof(C53A)=Sof(H53C)=Sof(H53D)=Sof(Cl1A)=1-FVAR(2)
 Sof(Cl1)=Sof(Cl2)=Sof(C53)=Sof(H53A)=Sof(H53B)=FVAR(2)
 Fixed Sof: O4(0.5) O4A(0.5) H35A(0.5) H35B(0.5) H35C(0.5) H35D(0.5) P2(0.5)
 F4(0.5) F4A(0.5) F5(0.5) F5A(0.5) F6(0.5) F6A(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C9(H9A,H9B), C10(H10A,H10B), C28(H28A,H28B),
 C29(H29A,H29B), C35(H35A,H35B), C35(H35C,H35D), C36(H36A,H36B), C53(H53A,H53B),
  C53A(H53C,H53D)
5.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C16(H16), C18(H18), C37(H37), C39(H39), C42(H42), C44(H44)
5.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C46(H46A,H46B,H46C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C),
 C52(H52A,H52B,H52C)
;
_shelx_res_checksum              39451
_shelx_hkl_checksum              35376
_olex2_submission_special_instructions 'No special instructions were received'