#------------------------------------------------------------------------------
#$Date: 2020-10-06 10:28:57 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257376 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/86/1558607.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_1558607
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         '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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -63.00 -36.00   1.00    5.00    --   10.87 -77.00 -60.00   27
  2  ω     44.00  69.00   1.00    5.00    --   10.87-178.00 150.00   25
  3  ω    -20.00  42.00   1.00    5.00    --   10.87 -99.00  60.00   62
  4  ω    -84.00  11.00   1.00    5.00    --  -11.58 -57.00 150.00   95
  5  ω    -15.00  15.00   1.00    5.00    --  -11.58 -99.00  60.00   30
  6  ω    -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       'ω 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/[σ²(Fo²)+(0.0333P)²+0.1594P] where P=(Fo²+2Fc²)/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 > 2σ(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_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   0.937
_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)
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Cr1 Cr 0.500000 0.000000 1.000000 0.0192(2) Uani 1 2 d S T P . .
O2 O 0.6472(3) 0.1827(2) 0.9906(2) 0.0186(5) Uani 1 1 d . . . . .
O1 O 0.4163(3) 0.1227(3) 1.1675(2) 0.0195(5) Uani 1 1 d . . . . .
N2 N -0.1275(4) 0.2080(3) 0.5841(3) 0.0248(7) Uani 1 1 d . . . . .
N1 N 0.2942(4) 0.0731(3) 0.8614(3) 0.0197(6) Uani 1 1 d . . . . .
C5 C 0.7873(5) 0.4458(4) 1.0481(4) 0.0288(9) Uani 1 1 d . . . . .
H5A H 0.900425 0.417765 1.084618 0.043 Uiso 1 1 calc GR . . . .
H5B H 0.773496 0.552986 1.100520 0.043 Uiso 1 1 calc GR . . . .
H5C H 0.771434 0.441418 0.944068 0.043 Uiso 1 1 calc GR . . . .
C8 C 0.0095(4) 0.1649(4) 0.6740(3) 0.0193(7) Uani 1 1 d . . . . .
C7 C -0.0063(5) 0.1120(4) 0.8024(3) 0.0239(8) Uani 1 1 d . . . . .
H7 H -0.112843 0.104932 0.827011 0.029 Uiso 1 1 calc R . . . .
C11 C -0.2999(5) 0.1783(4) 0.6044(4) 0.0286(9) Uani 1 1 d . . . . .
H11A H -0.315517 0.070648 0.616983 0.043 Uiso 1 1 calc GR . . . .
H11B H -0.381564 0.190175 0.518790 0.043 Uiso 1 1 calc GR . . . .
H11C H -0.316743 0.254291 0.690776 0.043 Uiso 1 1 calc GR . . . .
C12 C -0.1038(5) 0.2687(4) 0.4560(3) 0.0316(9) Uani 1 1 d . . . . .
H12A H -0.013937 0.355060 0.487540 0.047 Uiso 1 1 calc GR . . . .
H12B H -0.208637 0.307746 0.413253 0.047 Uiso 1 1 calc GR . . . .
H12C H -0.073333 0.183100 0.383448 0.047 Uiso 1 1 calc GR . . . .
C9 C 0.1751(5) 0.1700(4) 0.6466(3) 0.0233(8) Uani 1 1 d . . . . .
H9 H 0.195006 0.205440 0.565087 0.028 Uiso 1 1 calc R . . . .
C2 C 0.4408(4) 0.2791(4) 1.2164(3) 0.0197(8) Uani 1 1 d . . . . .
C6 C 0.1343(4) 0.0717(4) 0.8896(3) 0.0230(8) Uani 1 1 d . . . . .
H6 H 0.119964 0.040850 0.974765 0.028 Uiso 1 1 calc R . . . .
C10 C 0.3086(4) 0.1227(4) 0.7399(3) 0.0201(7) Uani 1 1 d . . . . .
H10 H 0.416273 0.125477 0.716961 0.024 Uiso 1 1 calc R . . . .
C3 C 0.5554(5) 0.3776(4) 1.1759(3) 0.0212(8) Uani 1 1 d . . . . .
H3 H 0.566402 0.486855 1.222545 0.025 Uiso 1 1 calc R . . . .
C1 C 0.3313(5) 0.3491(4) 1.3235(4) 0.0303(9) Uani 1 1 d . . . . .
H1A H 0.212408 0.329264 1.273964 0.045 Uiso 1 1 calc GR . . . .
H1B H 0.360930 0.463273 1.358778 0.045 Uiso 1 1 calc GR . . . .
H1C H 0.350780 0.299250 1.405937 0.045 Uiso 1 1 calc GR . . . .
C4 C 0.6564(4) 0.3287(4) 1.0716(3) 0.0204(8) Uani 1 1 d . . . . .
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'
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'
Cr Cr 0.3209 0.6236 '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
O2 Cr1 O2 180.0 2_657 . ?
O2 Cr1 O1 93.49(9) . . ?
O2 Cr1 O1 86.51(9) . 2_657 ?
O2 Cr1 O1 86.51(9) 2_657 . ?
O2 Cr1 O1 93.49(9) 2_657 2_657 ?
O2 Cr1 N1 89.80(9) . 2_657 ?
O2 Cr1 N1 90.20(9) . . ?
O2 Cr1 N1 89.80(9) 2_657 . ?
O2 Cr1 N1 90.20(9) 2_657 2_657 ?
O1 Cr1 O1 180.0 . 2_657 ?
O1 Cr1 N1 87.35(9) 2_657 2_657 ?
O1 Cr1 N1 92.65(9) 2_657 . ?
O1 Cr1 N1 87.35(9) . . ?
O1 Cr1 N1 92.65(9) . 2_657 ?
N1 Cr1 N1 180.0 2_657 . ?
C4 O2 Cr1 125.7(2) . . ?
C2 O1 Cr1 124.5(2) . . ?
C8 N2 C11 120.4(3) . . ?
C8 N2 C12 120.1(3) . . ?
C11 N2 C12 119.2(3) . . ?
C6 N1 Cr1 121.3(2) . . ?
C10 N1 Cr1 123.5(2) . . ?
C10 N1 C6 115.2(3) . . ?
N2 C8 C7 122.0(3) . . ?
N2 C8 C9 122.6(3) . . ?
C9 C8 C7 115.4(3) . . ?
C6 C7 C8 119.9(3) . . ?
C10 C9 C8 120.2(3) . . ?
O1 C2 C3 124.7(3) . . ?
O1 C2 C1 114.3(3) . . ?
C3 C2 C1 121.0(3) . . ?
N1 C6 C7 124.7(3) . . ?
N1 C10 C9 124.5(3) . . ?
C2 C3 C4 126.4(3) . . ?
O2 C4 C5 115.1(3) . . ?
O2 C4 C3 124.0(3) . . ?
C3 C4 C5 120.9(3) . . ?
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
Cr1 O2 1.947(2) 2_657 ?
Cr1 O2 1.947(2) . ?
Cr1 O1 1.949(2) 2_657 ?
Cr1 O1 1.949(2) . ?
Cr1 N1 2.096(3) . ?
Cr1 N1 2.096(3) 2_657 ?
O2 C4 1.299(4) . ?
O1 C2 1.305(4) . ?
N2 C8 1.361(4) . ?
N2 C11 1.450(4) . ?
N2 C12 1.465(4) . ?
N1 C6 1.357(4) . ?
N1 C10 1.338(4) . ?
C5 C4 1.502(5) . ?
C8 C7 1.417(4) . ?
C8 C9 1.401(5) . ?
C7 C6 1.358(5) . ?
C9 C10 1.376(5) . ?
C2 C3 1.387(4) . ?
C2 C1 1.511(4) . ?
C3 C4 1.402(4) . ?
