Manganese-promoted cleavage of acetylacetonate resembling the β-diketone cleaving dioxygenase (Dke1) reactivity.
Yang, Chao; Liu, Dingqi; Wang, Tongshuai; Sun, Fuxing; Qiu, Shilun; Wu, Gang; Chemical communications (Cambridge, England) 57 (2021) 9462–9465; doi:10.1039/d1cc02774c

data_7128868
_publ_section_title
;
 Manganese-promoted cleavage of acetylacetonate resembling the \b-diketone
 cleaving dioxygenase (Dke1) reactivity.
;
_journal_issue                   74
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9462
_journal_page_last               9465
_journal_paper_doi               10.1039/d1cc02774c
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C46 H41 Mn3 N4 O10, [+ solvents]'
_chemical_formula_sum            'C46 H41 Mn3 N4 O10'
_chemical_formula_weight         974.65
_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             2021-07-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-20 deposited with the CCDC.	2021-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.393(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.833(2)
_cell_length_b                   37.692(8)
_cell_length_c                   11.684(3)
_cell_measurement_reflns_used    5884
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      23.83
_cell_measurement_theta_min      2.38
_cell_volume                     4769.4(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1166
_diffrn_reflns_av_unetI/netI     0.0713
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            53128
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.119
_diffrn_reflns_theta_max         25.119
_diffrn_reflns_theta_min         2.381
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.840
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         8461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0917P)^2^+3.0676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1556
_refine_ls_wR_factor_ref         0.1717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5765
_reflns_number_total             8461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02774c2.cif
_cod_data_source_block           dke1-c3
_cod_depositor_comments
'Adding full bibliography for 7128866--7128868.cif.'
_cod_original_cell_volume        4769.1(17)
_cod_database_code               7128868
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.891
_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:
 C13(H13), C16(H16), C33(H33), C3(H3), C23(H23), C30(H30), C32(H32), C14(H14),
 C31(H31), C6(H6), C44(H44), C15(H15), C22(H22), C8(H8), C5(H5), C39(H39),
 C4(H4), C20(H20), C24(H24), C11(H11), C21(H21), C9(H9), C10(H10), C26(H26),
 C28(H28), C27(H27)
2.b Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C46(H46A,H46B,H46C), C41(H41A,H41B,H41C), C37(H37A,H37B,
 H37C), C36(H36A,H36B,H36C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 382 electrons were 
found in a volume of 758\%A^3^ in 1 void per unit cell. 
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              21862
_shelx_hkl_checksum              25937
_shelx_fab_checksum              15644
_olex2_submission_special_instructions 'No special instructions were received'