TEMPO Coordination and Reactivity in Group 6; Pseudo-Pentagonal Planar (η2-TEMPO)2CrX (X = Cl, TEMPO)
Wolczanski, Peter T.; Kayser, Ann K.; Lancaster, Kyle; Bollmeyer, Melissa M.; Cundari, Thomas R.; MacMillan, Samantha N.; Chemical Communications  (2022) –; doi:10.1039/D2CC03838B

data_7130479
_publ_section_title
;
 TEMPO Coordination and Reactivity in Group 6; Pseudo-Pentagonal Planar
 (\h2-TEMPO)2CrX (X = Cl, TEMPO)
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03838B
_journal_year                    2022
_chemical_formula_moiety         'C27 H54 Cr N3 O3'
_chemical_formula_sum            'C27 H54 Cr N3 O3'
_chemical_formula_weight         520.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-07
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2022-02-23 deposited with the CCDC.	2022-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                100.0300(10)
_cell_angle_beta                 93.7780(10)
_cell_angle_gamma                106.5100(10)
_cell_formula_units_Z            2
_cell_length_a                   9.75440(10)
_cell_length_b                   10.23250(10)
_cell_length_c                   15.2956(2)
_cell_measurement_reflns_used    19302
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      76.9030
_cell_measurement_theta_min      2.9440
_cell_volume                     1430.56(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -18.00  22.00   0.50    0.07    --   50.09 -19.00-120.00   80
  2  \w     32.00  66.00   0.50    0.27    --  104.00 -61.00 -90.00   68
  3  \w     73.00  99.00   0.50    0.27    --  104.00 -77.00-120.00   52
  4  \w     79.00 106.00   0.50    0.27    --  104.00 -79.00-155.55   54
  5  \w     70.00  96.00   0.50    0.27    --  104.00-125.00-150.00   52
  6  \w     61.00  87.00   0.50    0.27    --  104.00-125.00-180.00   52
  7  \w     43.00 106.00   0.50    0.27    --  104.00 -94.00-180.00  126
  8  \w     37.00  72.00   0.50    0.27    --  104.00 -94.00-120.00   70
  9  \w     61.00 105.00   0.50    0.27    --  104.00 -77.00 -60.00   88
 10  \w     79.00 106.00   0.50    0.27    --  104.00 -94.00 -30.00   54
 11  \w     81.00 106.00   0.50    0.27    --  104.00 -77.00   0.00   50
 12  \w     81.00 106.00   0.50    0.27    --  104.00 -94.00   0.00   50
 13  \w     80.00 112.00   0.50    0.27    --  104.00-125.00 -30.00   64
 14  \w     89.00 132.00   0.50    0.27    --  104.00-156.00 -17.00   86
 15  \w     83.00 108.00   0.50    0.27    --  104.00-113.00 -41.93   50
 16  \w     87.00 112.00   0.50    0.27    --  104.00-125.00 -60.00   50
 17  \w     86.00 129.00   0.50    0.27    --  104.00-157.00 -50.88   86
 18  \w     73.00  99.00   0.50    0.07    --   50.09-156.00 -17.00   52
 19  \w     63.00  89.00   0.50    0.27    --  104.00 -76.00 -19.12   52
 20  \w     67.00  93.00   0.50    0.27    --  104.00 -94.00 -60.00   52
 21  \w     50.00  76.00   0.50    0.27    --  104.00-125.00 -30.00   52
 22  \w     54.00  92.00   0.50    0.27    --  104.00-125.00   0.00   76
 23  \w     51.00  79.00   0.50    0.27    --  104.00-157.00 -50.88   56
 24  \w     32.00  64.00   0.50    0.27    --  104.00 -94.00 -30.00   64
 25  \w     33.00  63.00   0.50    0.27    --  104.00 -61.00 -30.00   60
 26  \w     32.00  71.00   0.50    0.27    --  104.00 -61.00  30.00   78
 27  \w     36.00  62.00   0.50    0.27    --  104.00 -77.00   0.00   52
 28  \w     33.00  58.00   0.50    0.27    --  104.00 -94.00  30.00   50
 29  \w     35.00  71.00   0.50    0.27    --  104.00 -61.00  60.00   72
 30  \w     81.00 106.00   0.50    0.27    --  104.00 -99.00 112.45   50
 31  \w     71.00  97.00   0.50    0.27    --  104.00-119.00 138.00   52
 32  \w     71.00 106.00   0.50    0.27    --  104.00 -94.00 120.00   70
 33  \w     51.00 112.00   0.50    0.27    --  104.00-125.00 120.00  122
 34  \w     42.00  91.00   0.50    0.07    --   50.09-119.00 138.00   98
 35  \w     35.00  61.00   0.50    0.27    --  104.00 -99.00 112.45   52
 36  \w     32.00  78.00   0.50    0.27    --  104.00 -77.00 120.00   92
 37  \w     41.00  66.00   0.50    0.27    --  104.00-125.00  60.00   50
 38  \w     34.00  90.00   0.50    0.27    --  104.00-125.00  90.00  112
 39  \w     33.00  71.00   0.50    0.27    --  104.00 -61.00 120.00   76
 40  \w     32.00  64.00   0.50    0.27    --  104.00 -61.00  90.00   64
 41  \w    114.00 157.00   0.50    0.27    --  104.00  15.00 150.00   86
 42  \w    140.00 166.00   0.50    0.27    --  104.00  30.00  60.00   52
 43  \w    148.00 174.00   0.50    0.27    --  104.00  30.00  30.00   52
 44  \w    151.00 176.00   0.50    0.27    --  104.00  61.00   0.00   50
 45  \w    138.00 171.00   0.50    0.27    --  104.00  30.00   0.00   66
 46  \w    139.00 164.00   0.50    0.27    --  104.00  15.00  30.00   50
 47  \w    110.00 136.00   0.50    0.27    --  104.00  30.00  30.00   52
 48  \w     99.00 131.00   0.50    0.27    --  104.00  30.00   0.00   64
 49  \w     92.00 118.00   0.50    0.27    --  104.00  61.00   0.00   52
 50  \w    103.00 149.00   0.50    0.27    --  104.00 112.00  62.96   92
 51  \w    148.00 176.00   0.50    0.27    --  104.00 125.00  60.00   56
 52  \w    131.00 157.00   0.50    0.27    --  104.00 125.00 -30.00   52
 53  \w    139.00 171.00   0.50    0.27    --  104.00 125.00 -90.00   64
 54  \w    147.00 172.00   0.50    0.27    --  104.00 125.00-150.00   50
 55  \w    136.00 161.00   0.50    0.27    --  104.00 119.00-136.00   50
 56  \w    112.00 138.00   0.50    0.27    --  104.00  43.00-128.63   52
 57  \w    118.00 144.00   0.50    0.27    --  104.00  30.00-180.00   52
 58  \w    101.00 134.00   0.50    0.27    --  104.00  15.00-150.00   66
 59  \w     97.00 175.00   0.50    0.27    --  104.00  45.00 -90.00  156
 60  \w    115.00 141.00   0.50    0.27    --  104.00 156.00  19.00   52
 61  \w     97.00 134.00   0.50    0.27    --  104.00 125.00 -90.00   74
 62  \w     96.00 128.00   0.50    0.27    --  104.00 125.00 -30.00   64
 63  \w     74.00  99.00   0.50    0.07    --   50.09 156.00  19.00   50
 64  \w    148.00 175.00   0.50    0.27    --  104.00 125.00 150.00   54
 65  \w     35.00  68.00   0.50    0.27    --  104.00 -61.00-120.00   66
 66  \w     38.00  83.00   0.50    0.27    --  104.00 -94.00-150.00   90
 67  \w     33.00  67.00   0.50    0.27    --  104.00 -61.00-180.00   68
 68  \w     34.00  60.00   0.50    0.27    --  104.00 -77.00-180.00   52
 69  \w     78.00 110.00   0.50    0.27    --  104.00   0.00-120.00   64
 70  \w     96.00 176.00   0.50    0.27    --  104.00  45.00-120.00  160
 71  \w    100.00 155.00   0.50    0.27    --  104.00 125.00-180.00  110
 72  \w     35.00  61.00   0.50    0.27    --  104.00 -61.00   0.00   52
 73  \w     34.00  71.00   0.50    0.27    --  104.00-125.00 -60.00   74
 74  \w    -60.00 -32.00   0.50    0.07    --  -50.09 -77.00-180.00   56
 75  \w   -121.00 -52.00   0.50    0.07    --  -50.09-156.00 -17.00  138
 76  \w    -91.00 -37.00   0.50    0.07    --  -50.09 -77.00  30.00  108
 77  \w   -107.00 -78.00   0.50    0.27    --  -82.50-119.00 138.00   58
 78  \w   -122.00 -97.00   0.50    0.27    --  -82.50-156.00 -17.00   50
 79  \w   -119.00 -63.00   0.50    0.07    --  -50.09 -77.00-180.00  112
 80  \w   -128.00 -82.00   0.50    0.27    --  -82.50 -30.00-180.00   92
 81  \w    -64.00 -11.00   0.50    0.07    --  -50.09 119.00-136.00  106
 82  \w    -92.00 -67.00   0.50    0.07    --  -50.09 156.00  19.00   50
 83  \w    -93.00 -68.00   0.50    0.27    --  -82.50 156.00  19.00   50
 84  \w    -72.00 -47.00   0.50    0.27    --  -82.50 119.00-136.00   50
 85  \w    -23.00  22.00   0.50    0.07    --  -50.09  19.00 150.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0403566000
_diffrn_orient_matrix_UB_12      0.0348468000
_diffrn_orient_matrix_UB_13      0.1022585000
_diffrn_orient_matrix_UB_21      -0.0017426000
_diffrn_orient_matrix_UB_22      0.1505715000
_diffrn_orient_matrix_UB_23      0.0020337000
_diffrn_orient_matrix_UB_31      -0.1609801000
_diffrn_orient_matrix_UB_32      -0.0426302000
_diffrn_orient_matrix_UB_33      0.0126278000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30784
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.734
_diffrn_reflns_theta_min         2.956
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.522
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.400
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
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            'clear purple'
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       block
_exptl_crystal_F_000             570
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.147
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         5171
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0843P)^2^+0.4567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1285
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4913
_reflns_number_total             5171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03838b2.cif
_cod_data_source_block           rakk16_abs
_cod_database_code               7130479
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C27H54CrN3O3
_chemical_oxdiff_usercomment     'Crystallized from ether.'
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.62
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C15(H15A,
 H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C)
;
_shelx_res_checksum              97617
_shelx_hkl_checksum              59176
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.676
_oxdiff_exptl_absorpt_empirical_full_min 0.663