Long-lived, near-IR emission from Cr(iii) under ambient conditions
Sawicka, Natalia; Craze, Chloe J.; Horton, Peter N.; Coles, Simon J.; Richards, Emma; Pope, Simon J. A.; Chemical Communications  (2022) –; doi:10.1039/D2CC01434C

data_7129990
_publ_section_title
;
 Long-lived, near-IR emission from Cr(iii) under ambient conditions
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC01434C
_journal_year                    2022
_chemical_formula_moiety         'C36 H24 Cr N10, F6 P, 0.5(C4 H10 O)'
_chemical_formula_sum            'C38 H29 Cr F6 N10 O0.5 P'
_chemical_formula_weight         830.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-03-02 deposited with the CCDC.	2022-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.483(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2896(3)
_cell_length_b                   8.7251(2)
_cell_length_c                   32.9959(10)
_cell_measurement_reflns_used    11444
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.2020
_cell_measurement_theta_min      2.6680
_cell_volume                     3536.90(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_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      100(2)
_diffrn_detector                 'hybrid pixel array detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000HE'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.982
_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    -89.00  89.00   0.50    5.00    --    0.00  59.00 -30.00  356
  2  \w    -89.00  89.00   0.50    5.00    --    0.00   0.00-180.00  356
  3  \w   -179.00  -1.00   0.50   25.00    --  -90.00  10.00-120.00  356
  4  \w   -165.00 -96.00   0.50   25.00    --  -90.00  51.00  15.98  138
  5  \w   -179.00  -1.00   0.50   25.00    --  -90.00  57.00  57.92  356
  6  \w   -179.00  -1.00   0.50   25.00    --  -90.00  39.00-150.00  356
  7  \w   -165.00  -8.00   0.50   25.00    --  -90.00  51.00  15.98  314
  8  \w    -45.00  -8.00   0.50   25.00    --  -90.00  51.00  15.98   74
  9  \w    -65.00 -27.00   0.50   25.00    --  -90.00  59.00 -50.35   76
 10  \w   -173.00 -72.00   0.50   25.00    --  -90.00  59.00 -50.35  202
 11  \w   -178.00 -88.00   0.50   25.00    --  -90.00  57.00  32.78  180
 12  \w    -89.00 -30.00   0.50    5.00    --    0.00  59.00-150.00  118
 13  \w    -89.00  89.00   0.50    5.00    --    0.00  39.00 -90.00  356
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter \c goniometer'
_diffrn_measurement_device_type
'Rigaku 007HF equipped with HF Varimax confocal mirrors and an AFC11 goniometer and HyPix 6000HE detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1139588000
_diffrn_orient_matrix_UB_12      -0.0035785000
_diffrn_orient_matrix_UB_13      -0.0184003000
_diffrn_orient_matrix_UB_21      0.0515303000
_diffrn_orient_matrix_UB_22      0.0402317000
_diffrn_orient_matrix_UB_23      0.0416923000
_diffrn_orient_matrix_UB_31      0.0096482000
_diffrn_orient_matrix_UB_32      -0.1719002000
_diffrn_orient_matrix_UB_33      0.0101352000
_diffrn_radiation_collimation    'HF Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            9714
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.606
_diffrn_reflns_theta_min         2.679
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    3.787
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
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    1.560
_exptl_crystal_description       needle
_exptl_crystal_F_000             1696
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of ether, toluene and MeCN'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.913
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         9714
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0894
_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^)+(0.1397P)^2^+19.0134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2486
_refine_ls_wR_factor_ref         0.2576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7915
_reflns_number_total             9714
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9836\% 
around [-0.00 -0.00 1.00] (reciprocal) or [0.07 -0.00 1.00] (direct)
;
_cod_data_source_file            d2cc01434c2.cif
_cod_data_source_block           '[Cr(bpi-1)2]PF6'
_cod_original_formula_sum        'C38 H29 Cr F6 N10 O0.50 P'
_cod_database_code               7129990
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C36 H24 Cr F6 N10 P'
_chemical_oxdiff_usercomment     NKS167
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.619
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.665(2)
 0.335(2)
2. 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
3. Rigid body (RIGU) restrains
 C54, C53, O51, C51, C52
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O51(0.5) C51(0.5) H51A(0.5) H51B(0.5) C52(0.5) H52A(0.5) H52B(0.5)
 H52C(0.5) C53(0.5) H53A(0.5) H53B(0.5) C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C53(H53A,H53B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C15(H15),
 C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24), C28(H28),
  C29(H29), C30(H30), C31(H31), C35(H35), C36(H36), C37(H37), C38(H38)
5.c Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              40717
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id NKS167
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.925
_oxdiff_exptl_absorpt_empirical_full_min 0.523
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2