Fluoro[η3-hydrotris(3-R-5-methylpyrazol-1-yl)borato]zinc(II): The First TpZnF Complexes, Convenient Precursors to Zinc Hydride Complexes,
Wolfgang Kläui; Uwe Schilde; Michael Schmidt; Inorganic Chemistry 36 (1997) 1598–1601; doi:10.1021/ic961249d

data_4323387
_publ_contact_author
;
 Schilde, Uwe
 Universit\"at Potsdam
 Institut f\"r Anorganische Chemie und Didaktik der Chemie
 Postfach 60 15 53
 Am Neuen Palais 10
 144 15 Potsdam
 Bundesrepublik Deutschland
;
_publ_contact_author_email       us@conrad.chem.uni-potsdam.de
_publ_section_title
;
 Fluoro[\h3-hydrotris(3-R-5-methylpyrazol-1-yl)borato]zinc(II): The First
 TpZnF Complexes, Convenient Precursors to Zinc Hydride Complexes,
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1598
_journal_page_last               1601
_journal_paper_doi               10.1021/ic961249d
_journal_volume                  36
_journal_year                    1997
_chemical_formula_moiety         'C33 H34 B F N6 Zn'
_chemical_formula_sum            'C33 H34 B F N6 Zn'
_chemical_formula_weight         609.84
_chemical_melting_point          465
_chemical_name_systematic
(Fluoro)[\h^3^-hydrotris(3-tolyl-5-methylpyrazol-1-yl)borate]zinc(II)
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   11.8719(12)
_cell_length_b                   11.8719(12)
_cell_length_c                   37.051(3)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      16.7
_cell_measurement_theta_min      9.1
_cell_volume                     4522.4(7)
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Stoe STADI4 diffractometer'
_diffrn_measurement_method       'omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2946
_diffrn_reflns_theta_max         30.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.854
_exptl_absorpt_correction_type   'empirical with XABS2'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.443
_refine_diff_density_min         -1.203
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.022
_refine_ls_hydrogen_treatment    'riding; except the boron H'
_refine_ls_number_parameters     133
_refine_ls_number_reflns         1487
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_obs          0.0425
_refine_ls_shift/esd_max         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1271
_refine_ls_wR_factor_obs         0.0962
_reflns_number_observed          1491
_reflns_number_total             1491
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961249d.cif
_cod_data_source_block           C33H34BFN6Zn
_cod_depositor_comments
;
The following automatic conversions were performed:

'_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 (18 times).

'_geom_bond_publ_flag' value 'N'
changed to 'n' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (15
times).

'_geom_angle_publ_flag' value 'N' changed to 'n' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (31 time).

'_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
(26 times).

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

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+0.0000P] 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^)+(0.0625P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               4323387