Synthesis of Zinc, Copper, Nickel, Cobalt, and Iron Complexes Using Tris(pyrazolyl)methane Sulfonate Ligands: A Structural Model for N,N,O Binding in Metalloenzymes
Papish, Elizabeth T.; Taylor, Michael T.; Jernigan, Finith E.; Rodig, Michael J.; Shawhan, Robert R.; Yap, Glenn P. A.; Jové, Fernando A.; Inorganic Chemistry 45 (2006) 2242–2250; doi:10.1021/ic051579a

data_4331804
_publ_section_title
;
 Synthesis of Zinc, Copper, Nickel, Cobalt, and Iron Complexes Using
 Tris(pyrazolyl)methane Sulfonate Ligands:&#x00A0; A Structural Model for
 N,N,O Binding in Metalloenzymes
;
_journal_issue                   5
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2242
_journal_page_last               2250
_journal_paper_doi               10.1021/ic051579a
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C76 H108 N24 Na4 O12 S4'
_chemical_formula_weight         1770.06
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                114.180(4)
_cell_angle_beta                 91.834(4)
_cell_angle_gamma                119.222(4)
_cell_formula_units_Z            1
_cell_length_a                   13.920(5)
_cell_length_b                   14.223(5)
_cell_length_c                   14.960(5)
_cell_measurement_reflns_used    775
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      20.15
_cell_measurement_theta_min      2.00
_cell_volume                     2255.8(14)
_computing_cell_refinement       'SHELXTL, Sheldrick (2001)'
_computing_data_collection       'SMART, Bruker (2002)'
_computing_data_reduction        'SHELXTL, Sheldrick (2001)'
_computing_molecular_graphics    'SHELXTL, Sheldrick (2001)'
_computing_publication_material  'SHELXTL, Sheldrick (2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.797
_diffrn_measured_fraction_theta_max 0.797
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       \w
_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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0646
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12845
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.195
_exptl_absorpt_correction_T_max  0.9770
_exptl_absorpt_correction_T_min  0.9584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick (2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         8918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+0.7987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1388
_reflns_number_gt                6529
_reflns_number_total             8918
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051579asup2.cif
_cod_data_source_block           lizp002
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2255.8(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4331804