Small Molecule Chemistry of the Pyrazolylborate-Zinc Unit TpCum,MeZn
Michael Ruf; Heinrich Vahrenkamp; Inorganic Chemistry 35 (1996) 6571–6578; doi:10.1021/ic960335a

data_4323959
_publ_section_title
;
 Small Molecule Chemistry of the Pyrazolylborate-Zinc Unit TpCum,MeZn
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6571
_journal_page_last               6578
_journal_paper_doi               10.1021/ic960335a
_journal_volume                  35
_journal_year                    1996
_chemical_compound_source        Ethanol/Dichlormethane
_chemical_formula_sum            'C42 H51 B N6 O S2 Zn'
_chemical_formula_weight         796.19
_chemical_name_systematic
'Hydrotris(3-cumyl-5-methyl-pyrazol-1-yl) borato-zink-ethylxanthogenat'
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.90(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.420(2)
_cell_length_b                   22.423(4)
_cell_length_c                   20.144(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      10.4
_cell_volume                     4249.5(15)
_computing_cell_refinement       'NONIUS EXPRESS'
_computing_data_collection       'NONIUS EXPRESS'
_computing_data_reduction        'CADFOR, CADSEX (E. Keller, 1976, 1981)'
_computing_molecular_graphics    'SCHAKAL (E. Keller, 1992)'
_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  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8573
_diffrn_reflns_theta_max         26.31
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        90
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_T_max  None
_exptl_absorpt_correction_T_min  None
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_meas      1.21
_exptl_crystal_density_method    floating
_exptl_crystal_description       rod
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_all   1.108
_refine_ls_goodness_of_fit_obs   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         8081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_restrained_S_obs      1.075
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_obs          0.0409
_refine_ls_shift/esd_max         -0.069
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+3.4282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1216
_refine_ls_wR_factor_obs         0.0925
_reflns_number_observed          5241
_reflns_number_total             8091
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960335a_7.cif
_cod_data_source_block           r28
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'None' changed to 'none'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

'_geom_bond_publ_flag'
value 'Y' changed to 'y' according to the built-in table from CIF
Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29
(64 times).

'_geom_angle_publ_flag' value 'Y' changed to 'y'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (104 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+3.4282P] 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^)+(0.0384P)^2^+3.4282P] 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        4249.5(14)
_cod_database_code               4323959