Pyrazolylborate-Zinc Alkoxide Complexes. 1. Basic Properties, Methylations, and Heterocumulene Insertions
Horst Brombacher; Heinrich Vahrenkamp; Inorganic Chemistry 43 (2004) 6042–6049; doi:10.1021/ic049179v

data_4311579
_publ_section_title
;
 Pyrazolylborate-Zinc Alkoxide Complexes. 1. Basic Properties,
 Methylations, and Heterocumulene Insertions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6042
_journal_page_last               6049
_journal_paper_doi               10.1021/ic049179v
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C33 H33 B N6 O S2 Zn'
_chemical_formula_weight         669.95
_chemical_melting_point          164
_chemical_name_common            Tp(Ph,Me)ZnSC(S)OEt
_chemical_name_systematic
; 
Hydrotris(3-phenyl-5-methyl-pyrazol-1-yl)borato-zink-(O-ethyl)-dithiocarbonat
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.959(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.526(2)
_cell_length_b                   18.106(5)
_cell_length_c                   18.990(5)
_cell_measurement_temperature    569(2)
_cell_volume                     3263.1(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      569(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1002
_diffrn_reflns_av_sigmaI/netI    0.1151
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29549
_diffrn_reflns_theta_full        28.46
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.917
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       isometric
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         7947
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.1793
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1126P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1698
_refine_ls_wR_factor_ref         0.2357
_reflns_number_gt                3234
_reflns_number_total             7947
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049179vsi20040706_092342_3.cif
_cod_data_source_block           test16
_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        3263.2(14)
_cod_database_code               4311579