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_7130481
_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         'C18 H36 Cl Cr N2 O2'
_chemical_formula_sum            'C18 H36 Cl Cr N2 O2'
_chemical_formula_weight         399.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-22
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2022-02-23 deposited with the CCDC.	2022-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.19810(10)
_cell_length_b                   14.66290(10)
_cell_length_c                   27.4065(2)
_cell_measurement_reflns_used    19061
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      77.9840
_cell_measurement_theta_min      3.2270
_cell_volume                     4098.20(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_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      100.0(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_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    107.00 153.00   0.50    1.75    --  107.75  45.00 -90.00   92
  2  \w    103.00 150.00   0.50    1.75    --  107.75  30.00-120.00   94
  3  \w    102.00 142.00   0.50    1.75    --  107.75  15.00-150.00   80
  4  \w    137.00 178.00   0.50    1.75    --  107.75  78.00  15.55   82
  5  \w    119.00 145.00   0.50    1.75    --  107.75  77.00 150.00   52
  6  \w     97.00 163.00   0.50    1.75    --  107.75  30.00 150.00  132
  7  \w    123.00 149.00   0.50    1.75    --  107.75 125.00-150.00   52
  8  \w     47.00 105.00   0.50    1.75    --  107.75 -77.00  23.00  116
  9  \w     43.00  69.00   0.50    1.75    --  107.75 -77.00   0.00   52
 10  \w     44.00  71.00   0.50    1.75    --  107.75 -61.00  30.00   54
 11  \w     37.00  69.00   0.50    1.75    --  107.75 -61.00  90.00   64
 12  \w     73.00  99.00   0.50    1.75    --  107.75 -77.00 150.00   52
 13  \w     59.00  84.00   0.50    1.75    --  107.75 -77.00  90.00   50
 14  \w    -14.00  25.00   0.50    0.44    --   48.30 -19.00-150.00   78
 15  \w     96.00 122.00   0.50    1.75    --  107.75 -83.00 -91.72   52
 16  \w     36.00 111.00   0.50    1.75    --  107.75-125.00-120.00  150
 17  \w     75.00 109.00   0.50    1.75    --  107.75-114.00-118.14   68
 18  \w     39.00  64.00   0.50    1.75    --  107.75-114.00-118.14   50
 19  \w     55.00  87.00   0.50    1.75    --  107.75-146.00 -25.00   64
 20  \w     37.00  94.00   0.50    1.75    --  107.75 -94.00-120.00  114
 21  \w     44.00  70.00   0.50    1.75    --  107.75 -84.00 -47.93   52
 22  \w     49.00  74.00   0.50    1.75    --  107.75-125.00 140.00   50
 23  \w     42.00  67.00   0.50    1.75    --  107.75-106.00  62.92   50
 24  \w     91.00 127.00   0.50    1.75    --  107.75 -84.00 -47.93   72
 25  \w     34.00  62.00   0.50    0.44    --   48.30-125.00 140.00   56
 26  \w    -50.00 -24.00   0.50    1.75    --  -86.25  44.00  -8.00   52
 27  \w   -114.00 -39.00   0.50    0.44    --  -48.30 -44.00-159.00  150
 28  \w    -99.00 -73.00   0.50    0.44    --  -48.30-125.00-180.00   52
 29  \w   -118.00 -93.00   0.50    0.44    --  -48.30-125.00 -90.00   50
;
_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      -0.0087735000
_diffrn_orient_matrix_UB_12      -0.0046844000
_diffrn_orient_matrix_UB_13      0.0560591000
_diffrn_orient_matrix_UB_21      0.0831510000
_diffrn_orient_matrix_UB_22      -0.0877153000
_diffrn_orient_matrix_UB_23      -0.0003030000
_diffrn_orient_matrix_UB_31      0.1257985000
_diffrn_orient_matrix_UB_32      0.0576642000
_diffrn_orient_matrix_UB_33      0.0041091000
_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  0.0390
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            30256
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.304
_diffrn_reflns_theta_min         3.225
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.883
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.316
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.117a (Rigaku Oxford Diffraction, 2021)
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    1.296
_exptl_crystal_description       plate
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.241
_exptl_crystal_size_mid          0.208
_exptl_crystal_size_min          0.059
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         4352
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0393P)^2^+1.1257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0721
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4043
_reflns_number_total             4352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03838b2.cif
_cod_data_source_block           rakk26_abs
_cod_database_code               7130481
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C18H36ClCrN2O2
_chemical_oxdiff_usercomment     'Crystallized from hexanes.'
_shelx_estimated_absorpt_t_max   0.719
_shelx_estimated_absorpt_t_min   0.333
_reflns_odcompleteness_completeness 98.11
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     78.89
_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:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              42603
_shelx_hkl_checksum              41497
_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 1.308
_oxdiff_exptl_absorpt_empirical_full_min 0.828