The energy gap law for NIR-phosphorescent Cr(III) complexes.
Cheng, Yang; Yang, Qingqing; He, Jiang; Zou, Wenjie; Liao, Keyu; Chang, Xiaoyong; Zou, Chao; Lu, Wei; Dalton transactions (Cambridge, England : 2003) 52 (2023) 2561–2565; doi:10.1039/d2dt02872g

data_7711614
_publ_section_title
;
 The energy gap law for NIR-phosphorescent Cr(III) complexes.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2561
_journal_page_last               2565
_journal_paper_doi               10.1039/d2dt02872g
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C40 H32 Cr N10, F6 P, 0.5(C H4 O), 0.5(H2 O)'
_chemical_formula_sum            'C41.13 H37.51 Cr F6 N10 O1.63 P'
_chemical_formula_weight         894.93
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-07-19 deposited with the CCDC.	2022-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.640(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.9874(13)
_cell_length_b                   18.8599(12)
_cell_length_c                   21.5414(14)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.83
_cell_measurement_theta_min      2.22
_cell_volume                     7923.5(9)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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 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 0.997
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0702
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            99292
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.372
_diffrn_reflns_theta_min         2.088
_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    0.408
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1247 before and 0.0685 after correction.
The Ratio of minimum to maximum transmission is 0.8820.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       block
_exptl_crystal_F_000             3683
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.355
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.086
_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     1104
_refine_ls_number_reflns         19782
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1077
_refine_ls_R_factor_gt           0.0597
_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^)+(0.0591P)^2^+14.5755P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1330
_refine_ls_wR_factor_ref         0.1583
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12837
_reflns_number_total             19782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02872g2.cif
_cod_data_source_block           cxy1645_0m
_cod_depositor_comments
'Adding full bibliography for 7711611--7711615.cif.'
_cod_database_code               7711614
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.877
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 P1-F1 \\sim P1-F1A
 with sigma of 0.02
 P1-F5 \\sim P1-F5A
 with sigma of 0.02
 P1-F4 \\sim P1-F4A
 with sigma of 0.02
 P1-F2 \\sim P1-F2A
 with sigma of 0.02
 P1-F6 \\sim P1-F6A
 with sigma of 0.02
 P1-F3 \\sim P1-F3A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
P1 \\sim F4A \\sim F6 \\sim F1A \\sim F5A \\sim F5 \\sim F2 \\sim F3 \\sim F1
\\sim F2A \\sim F4 \\sim F3A \\sim F6A: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(F2A) = Uanis(F2)
Uanis(F1A) = Uanis(F1)
Uanis(F6A) = Uanis(F6)
Uanis(F4) = Uanis(F4A)
Uanis(F5A) = Uanis(F5)
Uanis(F3A) = Uanis(F3)
4. Others
 Sof(F2A)=Sof(F3A)=Sof(F6A)=Sof(F5A)=Sof(F1A)=Sof(F4A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
5.a Free rotating group:
 O2(H2A,H2B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C15(H15), C23(H23), C13(H13), C26(H26), C12(H12), C24(H24), C40(H40),
 C35(H35), C32(H32), C39(H39), C18(H18), C37(H37), C19(H19), C20(H20), C38(H38),
  C6(H6), C4(H4), C33(H33), C17(H17), C72(H72), C43(H43), C80(H80), C44(H44),
 C63(H63), C53(H53), C79(H79), C55(H55), C73(H73), C52(H52), C64(H64), C60(H60),
  C66(H66), C75(H75), C46(H46), C58(H58), C59(H59), C57(H57), C77(H77), C78(H78)
5.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C7(H7A,H7B,H7C), C36(H36A,H36B,H36C), C27(H27A,H27B,
 H27C), C76(H76A,H76B,H76C), C47(H47A,H47B,H47C), C67(H67A,H67B,H67C), C56(H56A,
 H56B,H56C), C81(H81A,H81B,H81C)
5.d Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 84 electrons were 
found in a volume of 310\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.625[CH3OH] per Unit Cell 
which account for 90 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              45412
_shelx_fab_checksum              78
_olex2_submission_special_instructions 'No special instructions were received'