Ligand field-actuated redox-activity of acetylacetonate
Vinum, Morten Gotthold; Voigt, Laura; Hansen, Steen H.; Bell, Colby; Clark, Kensha Marie; Larsen, René Wugt; Pedersen, Kasper S.; Chemical Science 11 (2020) 8267–8272; doi:10.1039/D0SC01836H

data_1558607
_publ_section_title
;
 Ligand field-actuated redox-activity of acetylacetonate
;
_journal_issue                   31
_journal_name_full               'Chemical Science'
_journal_page_first              8267
_journal_page_last               8272
_journal_paper_doi               10.1039/D0SC01836H
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C24 H34 Cr N4 O4'
_chemical_formula_sum            'C24 H34 Cr N4 O4'
_chemical_formula_weight         494.55
_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     iterative
_audit_creation_date             2019-11-14
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-01 deposited with the CCDC.	2020-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                103.054(8)
_cell_angle_beta                 101.710(8)
_cell_angle_gamma                92.188(7)
_cell_formula_units_Z            1
_cell_length_a                   7.9894(7)
_cell_length_b                   8.5405(8)
_cell_length_c                   9.4779(9)
_cell_measurement_reflns_used    1227
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      24.1840
_cell_measurement_theta_min      4.0920
_cell_volume                     614.49(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3073
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_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    -63.00 -36.00   1.00    5.00    --   10.87 -77.00 -60.00   27
  2  \w     44.00  69.00   1.00    5.00    --   10.87-178.00 150.00   25
  3  \w    -20.00  42.00   1.00    5.00    --   10.87 -99.00  60.00   62
  4  \w    -84.00  11.00   1.00    5.00    --  -11.58 -57.00 150.00   95
  5  \w    -15.00  15.00   1.00    5.00    --  -11.58 -99.00  60.00   30
  6  \w    -39.00  55.00   1.00    5.00    --  -11.58  57.00 -60.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0740873000
_diffrn_orient_matrix_UB_12      -0.0551540000
_diffrn_orient_matrix_UB_13      -0.0301156000
_diffrn_orient_matrix_UB_21      -0.0373924000
_diffrn_orient_matrix_UB_22      0.0540887000
_diffrn_orient_matrix_UB_23      -0.0416008000
_diffrn_orient_matrix_UB_31      0.0373864000
_diffrn_orient_matrix_UB_32      -0.0368451000
_diffrn_orient_matrix_UB_33      -0.0596388000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.1023
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5094
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.366
_diffrn_reflns_theta_min         3.427
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'reddish black'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       block
_exptl_crystal_F_000             262
_exptl_crystal_size_max          0.251
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.131
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0600
_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^)+(0.0333P)^2^+0.1594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1252
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1772
_reflns_number_total             2494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01836h2.cif
_cod_data_source_block           exp_1542_cr(acac)2_dmap
_cod_depositor_comments
;Adding full bibliography for 1558605--1558608.cif.

 Adding full bibliography for 1558605--1558608.cif.
;
_cod_database_code               1558607
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cr1 O4 N4 C24 H34'
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.884
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C6(H6), C10(H10), C3(H3)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              73565
_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 1.532
_oxdiff_exptl_absorpt_empirical_full_min 0.730