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_7130480
_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 Mo N2 O4'
_chemical_formula_sum            'C18 H36 Mo N2 O4'
_chemical_formula_weight         440.43
_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             2021-03-10
_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                90
_cell_angle_beta                 118.845(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0580(6)
_cell_length_b                   15.6515(5)
_cell_length_c                   12.1533(5)
_cell_measurement_reflns_used    8374
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      31.2750
_cell_measurement_theta_min      3.2320
_cell_volume                     2009.06(19)
_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(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.965
_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    -22.00  15.00   0.50    6.84    --   -4.59 -82.00 -69.00   74
  2  \w     13.00  41.00   0.50    6.84    --    4.12-118.00 -82.52   56
  3  \w    -20.00  31.00   0.50    6.84    --    4.12 -99.00-120.00  102
  4  \w    -20.00  14.00   0.50    6.84    --   -4.59 -99.00-180.00   68
  5  \w    -26.00   5.00   0.50    6.84    --   -4.59  82.00  52.00   62
;
_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      -0.0463047000
_diffrn_orient_matrix_UB_12      -0.0229118000
_diffrn_orient_matrix_UB_13      -0.0524201000
_diffrn_orient_matrix_UB_21      0.0414064000
_diffrn_orient_matrix_UB_22      -0.0015760000
_diffrn_orient_matrix_UB_23      -0.0261082000
_diffrn_orient_matrix_UB_31      0.0255546000
_diffrn_orient_matrix_UB_32      -0.0390372000
_diffrn_orient_matrix_UB_33      0.0318324000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12030
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.231
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.805
_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 yellow'
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.227
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.949
_refine_diff_density_min         -1.661
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         3960
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0213P)^2^+7.5917P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1095
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3689
_reflns_number_total             3960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03838b2.cif
_cod_data_source_block           rakk18_abs
_cod_original_cell_volume        2009.06(18)
_cod_database_code               7130480
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C18H36MoN2O4
_chemical_oxdiff_usercomment     'Crystallized from ether.'
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.862
_reflns_odcompleteness_completeness 95.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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              31916
_shelx_hkl_checksum              16011
_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 1.117
_oxdiff_exptl_absorpt_empirical_full_min 0.837