#------------------------------------------------------------------------------
#$Date: 2020-10-06 10:28:57 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257376 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/86/1558605.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1558605
loop_
_publ_author_name
'Vinum, Morten Gotthold'
'Voigt, Laura'
'Hansen, Steen H.'
'Bell, Colby'
'Clark, Kensha Marie'
'Larsen, René Wugt'
'Pedersen, Kasper S.'
_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         '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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -33.00  39.00   1.00   10.00    --   10.87 -57.00  60.00   72
  2  ω    -22.00   4.00   1.00   10.00    --   10.87  19.00 -60.00   26
  3  ω    -17.00  62.00   1.00   10.00    --  -11.58  38.00  30.00   79
  4  ω     -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       'ω 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/[σ²(Fo²)+(0.0244P)²+0.5762P] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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)
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr0A Cr 0.000000 0.000000 0.500000 0.01114(18) Uani 1 2 d S T P . .
O0AA O -0.17704(17) 0.0816(3) 0.53705(13) 0.0141(4) Uani 1 1 d . . . . .
O1AA O -0.03413(17) -0.2371(3) 0.55142(13) 0.0143(4) Uani 1 1 d . . . . .
N0AA N 0.0835(2) 0.0717(3) 0.64666(16) 0.0136(5) Uani 1 1 d . . . . .
C1AA C 0.2722(3) 0.1761(4) 0.7576(2) 0.0213(7) Uani 1 1 d . . . . .
H1AA H 0.359938 0.221695 0.763538 0.026 Uiso 1 1 calc R . . . .
C2AA C 0.0181(3) 0.0413(4) 0.7335(2) 0.0161(6) Uani 1 1 d . . . . .
H2AA H -0.069234 -0.005221 0.726214 0.019 Uiso 1 1 calc R . . . .
C C -0.2547(3) -0.1878(4) 0.6075(2) 0.0180(6) Uani 1 1 d . . . . .
H H -0.326791 -0.241214 0.637937 0.022 Uiso 1 1 calc R . . . .
C3AA C 0.0746(3) 0.0757(4) 0.8321(2) 0.0208(7) Uani 1 1 d . . . . .
H3AA H 0.025359 0.053130 0.889225 0.025 Uiso 1 1 calc R . . . .
C4AA C 0.2045(3) 0.1436(4) 0.8456(2) 0.0216(7) Uani 1 1 d . . . . .
H4AA H 0.244965 0.166709 0.911398 0.026 Uiso 1 1 calc R . . . .
C5AA C 0.2096(3) 0.1409(4) 0.6609(2) 0.0177(6) Uani 1 1 d . . . . .
H5AA H 0.256469 0.165905 0.602824 0.021 Uiso 1 1 calc R . . . .
C6AA C -0.1412(3) -0.2950(4) 0.59224(19) 0.0169(6) Uani 1 1 d . . . . .
C7AA C -0.3937(3) 0.0949(4) 0.6034(2) 0.0216(7) Uani 1 1 d . . . . .
H7AA H -0.370786 0.182186 0.655912 0.032 Uiso 1 1 calc GR . . . .
H7AB H -0.460637 0.014881 0.627074 0.032 Uiso 1 1 calc GR . . . .
H7AC H -0.429527 0.153492 0.541357 0.032 Uiso 1 1 calc GR . . . .
C8AA C -0.2685(2) -0.0087(4) 0.58091(19) 0.0143(6) Uani 1 1 d . . . . .
C9AA C -0.1370(3) -0.4879(4) 0.6222(2) 0.0212(7) Uani 1 1 d . . . . .
H9AA H -0.127069 -0.559583 0.561779 0.032 Uiso 1 1 calc GR . . . .
H9AB H -0.219653 -0.519254 0.652302 0.032 Uiso 1 1 calc GR . . . .
H9AC H -0.061489 -0.508442 0.671675 0.032 Uiso 1 1 calc GR . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O0AA Cr0A O0AA 180.0 . 3_556 ?
O0AA Cr0A N0AA 90.11(8) . 3_556 ?
O0AA Cr0A N0AA 89.89(8) 3_556 3_556 ?
O0AA Cr0A N0AA 89.89(8) . . ?
O0AA Cr0A N0AA 90.11(8) 3_556 . ?
O1AA Cr0A O0AA 88.73(8) 3_556 . ?
O1AA Cr0A O0AA 91.27(8) . . ?
O1AA Cr0A O0AA 91.27(8) 3_556 3_556 ?
O1AA Cr0A O0AA 88.73(8) . 3_556 ?
O1AA Cr0A O1AA 180.0 . 3_556 ?
O1AA Cr0A N0AA 90.47(8) . 3_556 ?
O1AA Cr0A N0AA 89.53(8) 3_556 3_556 ?
O1AA Cr0A N0AA 89.53(8) . . ?
O1AA Cr0A N0AA 90.47(8) 3_556 . ?
N0AA Cr0A N0AA 180.00(13) . 3_556 ?
C8AA O0AA Cr0A 127.81(19) . . ?
C6AA O1AA Cr0A 128.13(19) . . ?
C2AA N0AA Cr0A 122.03(18) . . ?
C5AA N0AA Cr0A 121.58(17) . . ?
C5AA N0AA C2AA 116.3(2) . . ?
C5AA C1AA C4AA 120.0(3) . . ?
N0AA C2AA C3AA 123.4(3) . . ?
C8AA C C6AA 125.7(3) . . ?
C2AA C3AA C4AA 119.8(3) . . ?
C3AA C4AA C1AA 117.4(3) . . ?
N0AA C5AA C1AA 123.1(2) . . ?
O1AA C6AA C 123.4(3) . . ?
O1AA C6AA C9AA 115.0(2) . . ?
C C6AA C9AA 121.6(3) . . ?
O0AA C8AA C 123.7(2) . . ?
O0AA C8AA C7AA 115.1(3) . . ?
C C8AA C7AA 121.2(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr0A O0AA 1.9467(17) 3_556 ?
Cr0A O0AA 1.9467(17) . ?
Cr0A O1AA 1.938(2) 3_556 ?
Cr0A O1AA 1.938(2) . ?
Cr0A N0AA 2.085(2) 3_556 ?
Cr0A N0AA 2.085(2) . ?
O0AA C8AA 1.294(3) . ?
O1AA C6AA 1.292(3) . ?
N0AA C2AA 1.355(3) . ?
N0AA C5AA 1.351(3) . ?
C1AA C4AA 1.385(4) . ?
C1AA C5AA 1.381(4) . ?
C2AA C3AA 1.380(4) . ?
C C6AA 1.406(4) . ?
C C8AA 1.392(4) . ?
C3AA C4AA 1.381(4) . ?
C6AA C9AA 1.499(4) . ?
C7AA C8AA 1.508(4) . ?
