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_1558605
_publ_section_title
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 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         'C20 H24 Cr N2 O4'
_chemical_formula_sum            'C20 H24 Cr N2 O4'
_chemical_formula_weight         408.41
_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     direct
_audit_creation_date             2019-10-29
_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                90
_cell_angle_beta                 94.152(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8861(8)
_cell_length_b                   7.5065(8)
_cell_length_c                   12.9438(10)
_cell_measurement_reflns_used    1334
_cell_measurement_temperature    119.99(10)
_cell_measurement_theta_max      26.8670
_cell_measurement_theta_min      3.7140
_cell_volume                     958.04(15)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3073
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.844
_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    -33.00  39.00   1.00   10.00    --   10.87 -57.00  60.00   72
  2  \w    -22.00   4.00   1.00   10.00    --   10.87  19.00 -60.00   26
  3  \w    -17.00  62.00   1.00   10.00    --  -11.58  38.00  30.00   79
  4  \w     -3.00  27.00   1.00   10.00    --  -11.58 -99.00 150.00   30
;
_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      0.0665053000
_diffrn_orient_matrix_UB_12      -0.0114171000
_diffrn_orient_matrix_UB_13      0.0235491000
_diffrn_orient_matrix_UB_21      -0.0081214000
_diffrn_orient_matrix_UB_22      -0.0937206000
_diffrn_orient_matrix_UB_23      -0.0029609000
_diffrn_orient_matrix_UB_31      0.0262646000
_diffrn_orient_matrix_UB_32      0.0000916000
_diffrn_orient_matrix_UB_33      -0.0495801000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_unetI/netI     0.0912
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.844
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5145
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.757
_diffrn_reflns_theta_min         3.156
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87970
_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            'blackish green'
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       prism
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.119
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         2308
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+0.5762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.1092
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1610
_reflns_number_total             2308
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01836h2.cif
_cod_data_source_block           exp_1506_cr(acac)2(py)2_100pfit
_cod_depositor_comments
;Adding full bibliography for 1558605--1558608.cif.

 Adding full bibliography for 1558605--1558608.cif.
;
_cod_original_cell_volume        958.04(14)
_cod_database_code               1558605
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cr1 C20 O4 N2 H24'
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.883
_reflns_odcompleteness_completeness 99.72
_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:
 C1AA(H1AA), C2AA(H2AA), C(H), C3AA(H3AA), C4AA(H4AA), C5AA(H5AA)
2.b Idealised Me refined as rotating group:
 C7AA(H7AA,H7AB,H7AC), C9AA(H9AA,H9AB,H9AC)
;
_shelx_res_checksum              61433
_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 1.079
_oxdiff_exptl_absorpt_empirical_full_min 0.898