Copper Complexes as Bioinspired Models for Lytic Polysaccharide Monooxygenases.
Concia, Alda Lisa; Beccia, Maria Rosa; Orio, Maylis; Ferre, Francine Terra; Scarpellini, Marciela; Biaso, Frédéric; Guigliarelli, Bruno; Réglier, Marius; Simaan, A. Jalila; Inorganic chemistry 56 (2017) 1023–1026; doi:10.1021/acs.inorgchem.6b02165

data_4345467
_publ_section_title
;
 Copper Complexes as Bioinspired Models for Lytic Polysaccharide
 Monooxygenases.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1023
_journal_page_last               1026
_journal_paper_doi               10.1021/acs.inorgchem.6b02165
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C12 H14 Cu N4, F6 P'
_chemical_formula_sum            'C12 H14 Cu F6 N4 P'
_chemical_formula_weight         422.78
_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   mixed
_audit_creation_date             2015-10-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                85.611(3)
_cell_angle_beta                 78.271(3)
_cell_angle_gamma                73.584(3)
_cell_formula_units_Z            2
_cell_length_a                   8.8213(3)
_cell_length_b                   9.0761(3)
_cell_length_c                   9.9917(4)
_cell_measurement_reflns_used    6611
_cell_measurement_temperature    223.00(10)
_cell_measurement_theta_max      71.9540
_cell_measurement_theta_min      4.5070
_cell_volume                     751.18(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      223.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
  1 omega  -39.00   -5.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.3333  -57.0000 -120.0000 34

  2 omega   11.00   44.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  -90.0000 33

  3 omega   32.00   84.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       37.3333 -125.0000    0.0000 52

  4 omega   49.00   80.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       37.3333  -99.0000    0.0000 31

  5 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165  -94.0000    0.0000 84

  6 omega   59.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165 -111.0000  -90.0000 55

  7 omega   37.00  102.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165 -111.0000 -180.0000 65

  8 omega   25.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165 -111.0000  -90.0000 30

  9 omega   32.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165  -94.0000   90.0000 66

 10 omega   45.00   85.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   52.0000  -17.3607 40

 11 omega   72.00  148.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   66.0000  -66.3491 76

 12 omega  115.00  149.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   68.0000  -35.7939 34

 13 omega  112.00  138.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165   77.0000  -30.0000 26

 14 omega  131.00  157.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165   77.0000    0.0000 26

 15 omega  128.00  177.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165  111.0000   60.0000 49

 16 omega  108.00  139.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165   45.0000  150.0000 31

 17 omega  100.00  177.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165   77.0000  150.0000 77

 18 omega  101.00  173.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165  111.0000  -30.0000 72

 19 omega  109.00  145.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   72.0000 -176.6790 36

 20 omega   99.00  145.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165   77.0000  -90.0000 46

 21 omega  140.00  176.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165   77.0000 -180.0000 36

 22 omega   79.00  120.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165   61.0000    0.0000 41

 23 omega   73.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165   61.0000   60.0000 25

 24 omega   77.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165   61.0000   30.0000 27

 25 omega   70.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165   77.0000    0.0000 26

 26 omega   71.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165   77.0000  -30.0000 25

 27 omega   73.00  176.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165   77.0000  -60.0000 103

 28 omega   74.00  101.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165   45.0000  150.0000 27

 29 omega   70.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165   77.0000  150.0000 26

 30 omega   72.00  101.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165   61.0000  150.0000 29

 31 omega   70.00  160.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165   77.0000   90.0000 90

 32 omega   71.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165   77.0000  -90.0000 25

 33 omega   71.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165   77.0000 -120.0000 107

 34 omega   74.00  150.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165   56.0000 -172.0000 76

 35 omega   70.00  147.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165   77.0000 -150.0000 77

 36 omega   70.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165   77.0000 -180.0000 26

 37 omega   45.00   91.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   72.0000 -176.6790 46

 38 omega   24.00   50.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   66.0000  -66.3491 26

 39 omega   26.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   68.0000  -35.7939 29

 40 omega   24.00   88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000   11.8559 64

 41 omega   71.00  141.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165   77.0000   60.0000 70

 42 omega   71.00  173.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5165   77.0000   30.0000 102

 43 omega   28.00  151.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   66.0000  134.1797 123

 44 omega   22.00   49.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   78.0000  169.6284 27

 45 omega   14.00   40.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   83.0000  110.5264 26

 46 omega   18.00   43.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   81.0000   59.0378 25

 47 omega    2.00   27.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   91.0000   47.1800 25

 48 omega    6.00   31.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   90.0000  109.4617 25

 49 omega   14.00   43.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   82.0000  -46.2020 29

 50 omega   19.00   46.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   81.0000 -110.6255 27

 51 omega    6.00   31.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   90.0000 -104.9088 25

 52 omega  -83.00  -33.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.3333  125.0000   60.0000 50

 53 omega  -83.00  -20.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.3333  125.0000 -180.0000 63

 54 omega -120.00  -40.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.3333  -57.0000 -120.0000 80

 55 omega -113.00  -73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.3333 -125.0000  -30.0000 40

 56 omega  -45.00    2.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.3333  -77.0000   90.0000 47

 57 omega -120.00  -74.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.3333 -125.0000  150.0000 46

 58 omega -129.00  -55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.3333  -77.0000   90.0000 74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1336757000
_diffrn_orient_matrix_UB_12      0.1469634000
_diffrn_orient_matrix_UB_13      0.0472130000
_diffrn_orient_matrix_UB_21      -0.1025172000
_diffrn_orient_matrix_UB_22      -0.0340766000
_diffrn_orient_matrix_UB_23      -0.0952960000
_diffrn_orient_matrix_UB_31      -0.0775147000
_diffrn_orient_matrix_UB_32      -0.0925499000
_diffrn_orient_matrix_UB_33      0.1161786000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10225
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.194
_diffrn_reflns_theta_min         4.521
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.759
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_description       prism
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2916
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0300
_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^)+(0.0389P)^2^+0.4648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2705
_reflns_number_total             2916
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02165_si_004.cif
_cod_data_source_block           pylcul
_cod_original_cell_volume        751.17(5)
_cod_database_code               4345467
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups
2. Others
 Fixed Sof: H5AA(0.5) H5AB(0.5) H5AC(0.5) H5BD(0.5) H5BE(0.5) H5BF(0.5)
3.a Riding coordinates:
 C5(H5AA,H5AB,H5AC,H5BD,H5BE,H5BF)
3.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10)
;
_olex2_submission_special_instructions 'No special instructions were received'