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_4345468
_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 H16 Cu N4 O, H2 O, 2(Cl O4)'
_chemical_formula_sum            'C12 H18 Cl2 Cu N4 O10'
_chemical_formula_weight         512.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date
;
'Mon Feb 02 19:42:15 2015'
;
_audit_creation_method
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_cell_angle_alpha                85.809(3)
_cell_angle_beta                 83.461(3)
_cell_angle_gamma                84.995(3)
_cell_formula_units_Z            2
_cell_length_a                   8.1405(3)
_cell_length_b                   10.3453(4)
_cell_length_c                   11.6756(4)
_cell_measurement_reflns_used    6365
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.3480
_cell_measurement_theta_min      3.8100
_cell_volume                     971.17(6)
_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)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega -129.00  -34.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -34.3416  178.0000 -180.0000 95

  2 omega -130.00   61.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -34.3416    0.0000   60.0000 191

  3 omega   57.00  131.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       34.3416  178.0000    0.0000 74

  4 omega   57.00  131.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       34.3416  178.0000  -90.0000 74

  5 omega   55.00  129.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       34.3416 -178.0000 -180.0000 74

  6 omega   57.00  131.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       34.3416  178.0000   90.0000 74

  7 omega   53.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       97.3802   30.0000  -90.0000 125

  8 omega  100.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       97.3802  111.0000  -90.0000 78

  9 omega   60.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       97.3802   61.0000  -30.0000 118

 10 omega    7.00  109.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       97.3802  -94.0000   60.0000 102

 11 omega   14.00   98.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       97.3802  -45.0000  -90.0000 84

 12 omega   57.00  151.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       97.3802  178.0000  -30.0000 94

 13 omega  100.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       97.3802  111.0000  150.0000 78

 14 omega   62.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       97.3802   45.0000 -180.0000 116

 15 omega    7.00  109.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       97.3802  -94.0000 -150.0000 102

 16 omega  100.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       97.3802  111.0000   90.0000 78

 17 omega   14.00   98.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       97.3802  -45.0000   30.0000 84

 18 omega   12.00  115.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       97.3802 -111.0000  -60.0000 103

 19 omega -126.00    5.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -34.3416  -77.0000  -30.0000 131

 20 omega -126.00    5.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -34.3416  -77.0000   60.0000 131

 21 omega   -3.00  119.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       34.3416   38.0000  120.0000 122

 22 omega   -5.00  126.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       34.3416   77.0000  -30.0000 131

 23 omega   -2.00  119.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       34.3416   57.0000 -180.0000 121

 24 omega   -5.00  126.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       34.3416   77.0000 -120.0000 131

 25 omega   53.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       97.3802   30.0000   90.0000 125

 26 omega   58.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       97.3802   77.0000  -90.0000 120

 27 omega   58.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       97.3802   77.0000    0.0000 120

 28 omega   58.00  145.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       97.3802   77.0000 -180.0000 87

 29 omega   60.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       97.3802   61.0000  120.0000 118
;
_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      0.1756573000
_diffrn_orient_matrix_UB_12      0.0435456000
_diffrn_orient_matrix_UB_13      -0.0362166000
_diffrn_orient_matrix_UB_21      -0.0675812000
_diffrn_orient_matrix_UB_22      0.0939716000
_diffrn_orient_matrix_UB_23      -0.0952807000
_diffrn_orient_matrix_UB_31      -0.0330653000
_diffrn_orient_matrix_UB_32      0.1082117000
_diffrn_orient_matrix_UB_33      0.0855619000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13096
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        66.212
_diffrn_reflns_theta_max         66.212
_diffrn_reflns_theta_min         3.819
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.690
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51242
_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            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_description
;
;
_exptl_crystal_F_000             522
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         3370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0483P)^2^+0.8668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3033
_reflns_number_total             3370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02165_si_002.cif
_cod_data_source_block           pymima
_cod_original_cell_volume        971.18(7)
_cod_database_code               4345468
_cell_oxdiff_angle_alpha         85.809(3)
_cell_oxdiff_angle_beta          83.461(3)
_cell_oxdiff_angle_gamma         84.995(3)
_cell_oxdiff_length_a            8.1405(3)
_cell_oxdiff_length_b            10.3453(4)
_cell_oxdiff_length_c            11.6756(4)
_cell_oxdiff_measurement_reflns_used 6365
_cell_oxdiff_volume              971.18(7)
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     62.30
_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) groups, All O(H,H) groups
2.a Riding coordinates:
 O1(H1A,H1B)
2.b Free rotating group:
 O2(H2C,H2D)
2.c Secondary CH2 refined with riding coordinates:
 C1(H1C,H1D), C2(H2A,H2B)
2.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11)
2.e Idealised Me refined with riding coordinates:
 C12(H12A,H12B,H12C)
;
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'