Zn-O2H3-Zn: a Coordination Mode of the Hydrolytic Zinc-Aqua Function and a Possible Structural Motif for Oligozinc Enzymes
Michael Ruf; Karl Weis; Heinrich Vahrenkamp; Journal of the American Chemical Society 118 (1996) 9288–9294; doi:10.1021/ja960629v

data_4117175
_publ_section_title
;
 Zn-O2H3-Zn: a Coordination Mode of the Hydrolytic Zinc-Aqua Function and
 a Possible Structural Motif for Oligozinc Enzymes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9288
_journal_page_last               9294
_journal_paper_doi               10.1021/ja960629v
_journal_volume                  118
_journal_year                    1996
_chemical_compound_source        Methanol
_chemical_formula_sum            'C57 H66 B2 Cl N18 O9.5 Zn2'
_chemical_formula_weight         1343.09
_chemical_melting_point          185
_chemical_name_systematic
;
Bis[Hydrotris(3-(3'-pyridyl)-5-methyl-pyrazole-1-yl)borato-zinc-hydroxide]
hydroperchlorate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   'geom; difmap H(11), H(21)'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                99.570(7)
_cell_angle_beta                 105.190(8)
_cell_angle_gamma                113.430(7)
_cell_formula_units_Z            2
_cell_length_a                   15.068(1)
_cell_length_b                   15.601(1)
_cell_length_c                   17.734(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      10.4
_cell_volume                     3515.1(5)
_computing_cell_refinement       'NONIUS EXPRESS'
_computing_data_collection       'NONIUS EXPRESS'
_computing_data_reduction        'CADFOR, CADSEX (E. Keller 1976, 1981)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       Nonius-Turbo-CAD4
_diffrn_measurement_method       Omega-2Theta
_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  0.0406
_diffrn_reflns_av_sigmaI/netI    0.1379
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12703
_diffrn_reflns_theta_max         24.94
_diffrn_reflns_theta_min         2.22
_diffrn_standards_interval_count 'Icr every 3600 s, OCR every 200 refl.'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.956
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_meas      1.24
_exptl_crystal_density_method    floating
_exptl_crystal_description       isometric
_exptl_crystal_F_000             1394
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.065
_refine_ls_goodness_of_fit_obs   1.037
_refine_ls_hydrogen_treatment    'Riding Model; Least square H(11), H(21)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         12231
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_restrained_S_obs      1.037
_refine_ls_R_factor_all          0.2066
_refine_ls_R_factor_obs          0.0678
_refine_ls_shift/esd_max         -0.164
_refine_ls_shift/esd_mean        0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0989P)^2^+11.1393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2651
_refine_ls_wR_factor_obs         0.1699
_reflns_number_observed          5881
_reflns_number_total             12262
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja960629v_2.cif
_cod_data_source_block           w23[ref.no:3b]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0989P)^2^+11.1393P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0989P)^2^+11.1393P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3515.1(4)
_cod_original_formula_sum        'C57 H66 B2 Cl N18 O9.50 Zn2'
_cod_database_code               4117175