Complexes of 2-hydroxy-5-methyl-1,4-benzoquinone as models for the 'TPQ-on' form of copper amine oxidases
Foster, Caroline L.; Liu, Xiaoming; Kilner, Colin A.; Thornton-Pett, Mark; Halcrow, Malcolm A.; Journal of the Chemical Society, Dalton Transactions  (2000) 4563–; doi:10.1039/b006700h

data_7010186
_publ_section_title
;
 Complexes of 2-hydroxy-5-methyl-1,4-benzoquinone as models for the
 'TPQ-on' form of copper amine oxidases
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4563
_journal_paper_doi               10.1039/b006700h
_journal_year                    2000
_chemical_formula_moiety         '[C52 H39 B Cl Cu N6 O3].0.8[C H2 Cl2]'
_chemical_formula_sum            'C52.8 H40.6 B Cl1.6 Cu N6 O3'
_chemical_formula_weight         938.22
_chemical_name_systematic
; 
[Hydrido-tris-(3,5-diphenylpyrazolyl)borato][2-hydroxy-5-methyl-
benzoquinonato]copper(II) dichloromethane solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.2020(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4602(4)
_cell_length_b                   15.9627(4)
_cell_length_c                   19.6781(4)
_cell_measurement_reflns_used    51153
_cell_measurement_temperature    150(2)
_cell_volume                     4716.0(2)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method
;
   Detector set at 30mm from sample with different 2theta offsets 
   1 degree phi exposures for chi=0 degree settings
   1 degree omega exposures for chi=90 degree settings
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            51153
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_T_max  0.8991
_exptl_absorpt_correction_T_min  0.8540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Using multiple and symmetry-related data measurements via the program SORTAV
 See R.H. Blessing, Acta Cryst (1995), A51, 33-38 
;
_exptl_crystal_colour            Maroon
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1930
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.124
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.0139(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         10761
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1167P)^2^+2.3601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1821
_refine_ls_wR_factor_ref         0.1954
_reflns_number_gt                8284
_reflns_number_total             10761
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b006700h.txt
_cod_data_source_block           clf53
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        4715.96(19)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C52.80 H40.6 B Cl1.60 Cu N6 O3'
_cod_database_code               7010186