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_7701902
_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_formula_moiety
'C37 H36 Cu2 N10 O3, 2(Cl O4), 0.5(C4 H10 O), 1.5(C2 H3 N)'
_chemical_formula_sum            'C42 H45.5 Cl2 Cu2 N11.5 O11.5'
_chemical_formula_weight         1093.38
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-07 deposited with the CCDC.
2018-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                80.111(2)
_cell_angle_beta                 71.250(2)
_cell_angle_gamma                61.8690(10)
_cell_formula_units_Z            2
_cell_length_a                   12.8864(8)
_cell_length_b                   13.1530(8)
_cell_length_c                   16.6060(11)
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.55
_cell_volume                     2349.7(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX 3 (Bruker, 2017) '
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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                 'CMOS area detector'
_diffrn_detector_area_resol_mean 5.12
_diffrn_detector_type            'Bruker PHOTON 50'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    '0.5 mm double-pinhole'
_diffrn_radiation_detector       'Bruker PHOTON 50'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            55045
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.434
_diffrn_reflns_theta_min         1.295
_diffrn_source                   'standard sealed X-ray tube'
_diffrn_source_type              'Siemens, KFF Mo 2K -90 C'
_exptl_absorpt_coefficient_mu    1.092
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0479 before and 0.0373 after correction. The Ratio of minimum to maximum transmission is 0.8954. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1124
_exptl_crystal_recrystallization_method
'crystallized fom a saturared acetonitrile solution'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.020
_refine_diff_density_min         -2.020
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         9654
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0658
_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^)+(0.0771P)^2^+12.1092P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1727
_refine_ls_wR_factor_ref         0.1770
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8734
_reflns_number_total             9654
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01378k2.cif
_cod_data_source_block           5
_cod_original_formula_sum        'C42 H45.50 Cl2 Cu2 N11.50 O11.50'
_cod_database_code               7701902
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.708
_olex2_refinement_description
;
1. 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
2. Restrained distances
 C67-C66 = C63-C64
 1.54 with sigma of 0.02
 O65-C64 = O65-C66
 1.4 with sigma of 0.01
 C66-C64
 1.7 with sigma of 0.01
 C64-C66
 1.75 with sigma of 0.001
 N62-C61
 1.15 with sigma of 0.01
 C60-C61
 1.54 with sigma of 0.01
 H43_$1-H64A
 2.1 with sigma of 0.01
 C64-C63 \\sim C67-C66
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C60) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(N62) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C56) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O2) = Uanis(O4) = Uanis(O1) = Uanis(O3)
Uanis(Cl3) = Uanis(Cl1)
Uanis(O10) = Uanis(O11) = Uanis(O12) = Uanis(O9)
Uanis(C63) = Uanis(C64) = Uanis(O65) = Uanis(C66) = Uanis(C67)
Uanis(N62) = Uanis(C61) = Uanis(C60)
4. Others
 1*[Sof(N54)+Sof(C55)+Sof(C56)+Sof(H56A)+Sof(H56B)+Sof(H56C)]+1*[Sof(N51)+
 Sof(C52)+Sof(C53)+Sof(H53A)+Sof(H53B)+Sof(H53C)]+1*[Sof(C57)+Sof(H57A)+
 Sof(H57B)+Sof(H57C)+Sof(C58)+Sof(N59)]+1*[Sof(C60)+Sof(H60A)+Sof(H60B)+
 Sof(H60C)+Sof(C61)+Sof(N62)]=1.5 with esd of 0.001
 Sof(Cl3)=Sof(O9)=Sof(O10)=Sof(O11)=Sof(O12)=1-FVAR(1)
 Sof(O1)=Sof(Cl1)=Sof(O2)=Sof(O3)=Sof(O4)=FVAR(1)
 Sof(N54)=Sof(C55)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=FVAR(2)
 Sof(N51)=Sof(C52)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=FVAR(3)
 Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(C58)=Sof(N59)=FVAR(4)
 Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=Sof(C61)=Sof(N62)=FVAR(5)
 Fixed Sof: C63(0.5) H63A(0.5) H63B(0.5) H63C(0.5) C64(0.5) H64A(0.5)
 H64B(0.5) O65(0.5) C66(0.5) H66A(0.5) H66B(0.5) C67(0.5) H67A(0.5) H67B(0.5)
 H67C(0.5)
5.a Ternary CH refined with riding coordinates:
 C23(H23)
5.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C20(H20A,H20B), C22(H22A,H22B), C25(H25A,H25B), C35(H35A,
 H35B), C45(H45A,H45B), C64(H64A,H64B), C66(H66A,H66B)
5.c Me refined with riding coordinates:
 C60(H60A,H60B,H60C)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), N8(H8), C13(H13), C14(H14), C15(H15),
 C16(H16), N18(H18), C28(H28), C29(H29), C30(H30), C31(H31), N33(H33), C38(H38),
  C39(H39), C40(H40), C41(H41), N43(H43)
5.e Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C63(H63A,H63B,H63C), C67(H67A,H67B,H67C), C57(H57A,H57B,
 H57C), C56(H56A,H56B,H56C), C53(H53A,H53B,H53C)
;
_shelx_res_checksum              61564
_olex2_exptl_crystal_mounting_method 'mounted in oil on a Mitegen holder'
_olex2_submission_original_sample_id DAN102a
_olex2_submission_special_instructions 'No special instructions were received'