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_7701903
_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 ad
_chemical_formula_moiety         'C42 H38 Cu2 N10 O3, 1.5(C2 H3 N), 2(Cl O4)'
_chemical_formula_sum            'C45 H42.5 Cl2 Cu2 N11.5 O11'
_chemical_formula_weight         1118.38
_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             2017-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_audit_update_record
;
2018-02-07 deposited with the CCDC.
2018-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.2580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.4647(8)
_cell_length_b                   21.8424(8)
_cell_length_c                   11.5893(4)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.46
_cell_measurement_theta_min      2.65
_cell_volume                     4827.9(3)
_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
_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 0.996
_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  0.0394
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            41111
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.547
_diffrn_reflns_theta_min         2.651
_diffrn_source                   'standard sealed x-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.064
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7002
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0651 before and 0.0572 after correction.
The Ratio of minimum to maximum transmission is 0.9394.
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    1.539
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2292
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.866
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.276(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         10007
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0606P)^2^+11.5017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1123
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                9189
_reflns_number_total             10007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01378k2.cif
_cod_data_source_block           4
_cod_original_formula_sum        'C45 H42.50 Cl2 Cu2 N11.50 O11'
_cod_database_code               7701903
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.724(15) 0.276(15)
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
 C60-C61 \\sim C58-C57
 with sigma of 0.01
 N56-C57 \\sim N59-C60
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(N59) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C61) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(Cl2A) \\sim Ueq, Uanis(Cl2) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O67A) = Uanis(O67) = Uanis(O66A) = Uanis(O66) = Uanis(O69) = Uanis(O69A)
= Uanis(O68)
Uanis(Cl2A) = Uanis(Cl2)
5. Others
 Sof(Cl2A)=Sof(O69A)=Sof(O66)=Sof(O67)=1-FVAR(1)
 Sof(Cl2)=Sof(O66A)=Sof(O67A)=Sof(O69)=FVAR(1)
 Fixed Sof: C60(0.5) C61(0.5) H61A(0.5) H61B(0.5) H61C(0.5) N59(0.5)
6.a Ternary CH refined with riding coordinates:
 C23(H23)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B), C22(H22A,H22B), C25(H25A,H25B), C37(H37A,
 H37B), C27(H27A,H27B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C16(H16), C17(H17), C18(H18), C19(H19),
 C31(H31), C32(H32), C33(H33), C34(H34), C41(H41), C42(H42), C43(H43), C44(H44),
  C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), N8(H8), N14(H14), N29(H29),
 N39(H39)
6.d Idealised Me refined as rotating group:
 C61(H61A,H61B,H61C), C58(H58A,H58B,H58C)
;
_shelx_res_checksum              48953
_olex2_exptl_crystal_mounting_method 'mounted in oil on a Mitegen holder'
_olex2_submission_original_sample_id DAN102b
_olex2_submission_special_instructions 'No special instructions were received'