Catechol oxidase activity of comparable dimanganese and dicopper complexes.
Magherusan, Adriana M.; Nelis, Daniel N.; Twamley, Brendan; McDonald, Aidan R.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 15555–15564; doi:10.1039/c8dt01378k

data_7701901
_publ_section_title
;
 Catechol oxidase activity of comparable dimanganese and dicopper
 complexes.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15555
_journal_page_last               15564
_journal_paper_doi               10.1039/c8dt01378k
_journal_volume                  47
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C42 H37 Mn2 N10 O3, 2(Cl O4), 2(C2 H3 N)'
_chemical_formula_sum            'C46 H43 Cl2 Mn2 N12 O11'
_chemical_formula_weight         1120.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-03-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2018-02-07 deposited with the CCDC.
2018-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.314(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.3934(11)
_cell_length_b                   21.7926(11)
_cell_length_c                   11.6260(6)
_cell_measurement_reflns_used    9030
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.70
_cell_measurement_theta_min      2.69
_cell_volume                     4899.8(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker D8 Quest ECO'
_diffrn_detector_area_resol_mean 5.12
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest ECO'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            68365
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.736
_diffrn_source                   'standard sealed x-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0873 before and 0.0660 after correction. The Ratio of minimum to maximum transmission is 0.9145. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       lozenge
_exptl_crystal_F_000             2300
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.722
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         9586
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0766
_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^)+(0.0308P)^2^+50.5236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.1703
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                7856
_reflns_number_total             9586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01378k2.cif
_cod_data_source_block           6
_cod_original_cell_volume        4899.8(4)
_cod_database_code               7701901
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.885
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51(5)
 0.49(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C25A-C36A
 2.3 with sigma of 0.01
 N21-C22 = N21-C22A
 1.45 with sigma of 0.01
 C23-C22 = C23-C22A
 1.52 with sigma of 0.01
 C25A-C23 = C25-C23
 1.52 with sigma of 0.01
 N26-C25A
 1.49 with sigma of 0.01
 N21-C22A \\sim N21-C22
 with sigma of 0.01
 N21-C10A \\sim N21-C10
 with sigma of 0.01
 N21-C20A \\sim N21-C10
 with sigma of 0.01
 C36A-C35 \\sim C36-C35
 with sigma of 0.01
 C10-C9 \\sim C10A-C9A
 with sigma of 0.01
 N8-C7A \\sim N8A-C7A
 with sigma of 0.01
 N8A-C9A \\sim N8-C9
 with sigma of 0.01
 N1A-C2A \\sim N1-C2A
 with sigma of 0.01
 N1-C2 \\sim N1A-C2A
 with sigma of 0.01
 N1-C9 \\sim N1A-C9A
 with sigma of 0.01
4. Restrained planarity
 N1A, C2A, C7A, C7A, N8A, C9A
 with sigma of 0.01
 N37A, C43A, C38A, N44A, C45A
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(C10) = Uanis(C10A) = Uanis(C20) = Uanis(C20A)
Uanis(C46A) = Uanis(C46) = Uanis(C25) = Uanis(C25A) = Uanis(C36) = Uanis(C36A)
Uanis(C22A) = Uanis(C22) = Uanis(C25A) = Uanis(C25)
Uanis(N37) = Uanis(N44) = Uanis(C41A) = Uanis(C40A) = Uanis(C39A) = Uanis(C38)
= Uanis(C43) = Uanis(C42A) = Uanis(C45) = Uanis(N44A) = Uanis(C45A) =
Uanis(N37A) = Uanis(C38A) = Uanis(C39) = Uanis(C40) = Uanis(C41) = Uanis(C42) =
Uanis(C43A)
Uanis(C7A) = Uanis(C2A) = Uanis(C6A) = Uanis(C5A) = Uanis(C4A) = Uanis(C3A) =
Uanis(C9) = Uanis(N8) = Uanis(N1) = Uanis(N8A) = Uanis(C9A) = Uanis(N1A) =
Uanis(C7) = Uanis(C3) = Uanis(C2) = Uanis(C4) = Uanis(C6) = Uanis(C5)
Uanis(O4) = Uanis(O4A) = Uanis(O3) = Uanis(O3A) = Uanis(O1) = Uanis(O1A) =
Uanis(O2) = Uanis(O2A)
Uanis(Cl1A) = Uanis(Cl1)
Uanis(O6) = Uanis(O6A) = Uanis(O5) = Uanis(O5A) = Uanis(O7) = Uanis(O7A) =
Uanis(O8) = Uanis(O8A)
Uanis(Cl2) = Uanis(Cl2A)
6. Others
 Sof(N1A)=Sof(N8A)=Sof(H8A)=Sof(N37A)=Sof(N44A)=Sof(H44A)=Sof(C3A)=Sof(H3A)=
 Sof(C2A)=Sof(C7A)=Sof(C6A)=Sof(H6A)=Sof(C5A)=Sof(H5A)=Sof(C4A)=Sof(H4A)=
 Sof(C9A)=Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(C22)=
 Sof(H22A)=Sof(H22B)=Sof(C25A)=Sof(H25C)=Sof(H25D)=Sof(C36A)=Sof(H36C)=
 Sof(H36D)=Sof(C43A)=Sof(C42A)=Sof(H42A)=Sof(C41A)=Sof(H41A)=Sof(C40A)=
 Sof(H40A)=Sof(C39A)=Sof(H39A)=Sof(C38A)=Sof(C45A)=Sof(C46A)=Sof(H46C)=
 Sof(H46D)=1-FVAR(1)
 Sof(N1)=Sof(N8)=Sof(H8)=Sof(N37)=Sof(N44)=Sof(H44)=Sof(C7)=Sof(C2)=Sof(C3)=
 Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C9)=Sof(C10)=
 Sof(H10A)=Sof(H10B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C22A)=Sof(H22C)=Sof(H22D)=
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C42)=Sof(H42)=
 Sof(C41)=Sof(H41)=Sof(C40)=Sof(H40)=Sof(C39)=Sof(H39)=Sof(C38)=Sof(C43)=
 Sof(C45)=Sof(C46)=Sof(H46A)=Sof(H46B)=FVAR(1)
 Sof(Cl1A)=Sof(O2A)=Sof(O4A)=Sof(O1A)=Sof(O3A)=1-FVAR(2)
 Sof(Cl1)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=FVAR(2)
 Sof(Cl2A)=Sof(O6A)=Sof(O7A)=Sof(O5A)=Sof(O8A)=1-FVAR(3)
 Sof(Cl2)=Sof(O5)=Sof(O6)=Sof(O7)=Sof(O8)=FVAR(3)
7.a Free rotating group:
 Cl1A(O2A,O4A,O1A,O3A), Cl2A(O6A,O7A,O5A,O8A)
7.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C10A(H10C,H10D), C20(H20A,H20B), C20A(H20C,H20D), C22(H22A,
 H22B), C22A(H22C,H22D), C25(H25A,H25B), C25A(H25C,H25D), C36(H36A,H36B),
 C36A(H36C,H36D), C46(H46A,H46B), C46A(H46C,H46D)
7.c Aromatic/amide H refined with riding coordinates:
 N8(H8), N8A(H8A), N18(H18), N34(H34), N44(H44), N44A(H44A), C3A(H3A),
 C6A(H6A), C5A(H5A), C4A(H4A), C3(H3), C4(H4), C5(H5), C6(H6), C13(H13),
 C14(H14), C15(H15), C16(H16), C29(H29), C30(H30), C31(H31), C32(H32), C42(H42),
  C41(H41), C40(H40), C39(H39), C42A(H42A), C41A(H41A), C40A(H40A), C39A(H39A),
 C51(H51), C52(H52), C53(H53), C54(H54), C55(H55)
7.d Fitted hexagon refined as free rotating group:
 C3A(C2A,C7A,C6A,C5A,C4A), C7(C2,C3,C4,C5,C6), C42(C41,C40,C39,C38,C43),
 C43A(C42A,C41A,C40A,C39A,C38A)
7.e Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C), C61(H61A,H61B,H61C)
;
_shelx_res_checksum              37739
_olex2_exptl_crystal_mounting_method 'mounted in oil on a Mitegen holder'
_olex2_submission_original_sample_id AMM636
_olex2_submission_special_instructions 'No special instructions were received'