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_4345469
_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         'C14 H19 Cu N5, 2(Cl O4)'
_chemical_formula_sum            'C14 H19 Cl2 Cu N5 O8'
_chemical_formula_weight         519.78
_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   geom
_audit_creation_date             2016-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.31 svn.r3340 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                84.583(2)
_cell_angle_beta                 79.429(3)
_cell_angle_gamma                83.371(3)
_cell_formula_units_Z            2
_cell_length_a                   8.8001(3)
_cell_length_b                   10.4679(3)
_cell_length_c                   11.3132(3)
_cell_measurement_reflns_used    4839
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.8280
_cell_measurement_theta_min      4.0400
_cell_volume                     1014.75(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)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
  1 omega  -42.00   40.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.5600   38.0000    0.0000 82

  2 omega   17.00   67.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       37.5600   38.0000 -150.0000 50

  3 omega   32.00   80.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.4555  -30.0000 -150.0000 48

  4 omega   46.00  126.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.4555  -77.0000 -150.0000 80

  5 omega   66.00  107.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.4555  -94.0000  -30.0000 41

  6 omega   75.00  108.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.4555  -94.0000   60.0000 33

  7 omega   41.00   90.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.4555  -30.0000  150.0000 49

  8 omega   75.00  145.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.4555   30.0000   60.0000 70

  9 omega   84.00  177.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.4555   45.0000  -30.0000 93

 10 omega  152.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.4555  111.0000 -120.0000 26

 11 omega  111.00  172.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.4555  111.0000 -180.0000 61

 12 omega  102.00  129.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.4555  111.0000 -120.0000 27

 13 omega  104.00  176.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.4555  111.0000  -90.0000 72

 14 omega   35.00   81.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.4555  -30.0000   30.0000 46

 15 omega   35.00   88.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.4555  -45.0000  -60.0000 53

 16 omega   38.00  115.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      112.4555 -111.0000 -150.0000 77

 17 omega   48.00   91.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       37.5600 -125.0000 -150.0000 43

 18 omega   23.00   80.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       37.5600 -125.0000   60.0000 57

 19 omega    8.00   48.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       37.5600  -99.0000   90.0000 40

 20 omega  -40.00   30.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       37.5600  -57.0000   90.0000 70

 21 omega -113.00   -5.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.5600  -57.0000 -150.0000 108
;
_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      -0.1777274000
_diffrn_orient_matrix_UB_12      0.0287052000
_diffrn_orient_matrix_UB_13      0.0130685000
_diffrn_orient_matrix_UB_21      0.0164254000
_diffrn_orient_matrix_UB_22      0.1457478000
_diffrn_orient_matrix_UB_23      -0.0102876000
_diffrn_orient_matrix_UB_31      0.0133936000
_diffrn_orient_matrix_UB_32      0.0030713000
_diffrn_orient_matrix_UB_33      -0.1379171000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0132
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6307
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.795
_diffrn_reflns_theta_min         3.986
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.438
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74123
_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    1.701
_exptl_crystal_description
;
;
_exptl_crystal_F_000             530
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4034
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.249
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0524P)^2^+0.4555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.0966
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3806
_reflns_number_total             4034
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02165_si_003.cif
_cod_data_source_block           pymim-acn
_cod_database_code               4345469
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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. Uiso/Uaniso restraints and constraints
Cl1 \\sim O1: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
3.a Ternary CH refined with riding coordinates:
 N1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C8(H8A,H8B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11)
3.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C)
;
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'