Methylation of (2-methylethanethiol-bis-3,5-dimethylpyrazolyl)methane zinc complexes and coordination of the resulting thioether: relevance to zinc-containing alkyl transfer enzymes
Hammes, Brian S.; Carrano, Carl J.; Chemical Communications  (2000) 1635–; doi:10.1039/b004338i

data_7111023
_publ_section_title
;
 Methylation of (2-methylethanethiol-bis-3,5-dimethylpyrazolyl)methane
 zinc complexes and coordination of the resulting thioether: relevance to
 zinc-containing alkyl transfer enzymes
;
_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1635
_journal_paper_doi               10.1039/b004338i
_journal_year                    2000
_chemical_formula_sum            'C15 H24 B F4 I N4 S Zn'
_chemical_formula_weight         571.52
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            9
_cell_length_a                   9.752(2)
_cell_length_b                   19.758(3)
_cell_length_c                   22.963(3)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.53
_cell_measurement_theta_min      5.16
_cell_volume                     4424.5(13)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2635
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         1.77
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.970
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_F_000             2538
_refine_diff_density_max         0.978
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.980
_refine_ls_goodness_of_fit_obs   0.992
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         2633
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.040
_refine_ls_restrained_S_obs      0.986
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_obs          0.0640
_refine_ls_shift/esd_max         0.275
_refine_ls_shift/esd_mean        0.019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1149P)^2^+33.5611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2200
_refine_ls_wR_factor_obs         0.1607
_reflns_number_observed          1639
_reflns_number_total             2635
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b004338isup1.cif
_cod_data_source_block           bsh70
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1149P)^2^+33.5611P] 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^)+(0.1149P)^2^+33.5611P] 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        4424.3(13)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7111023