Halocarbonyltungsten(II) Complexes Containing Tripodal Tris(pyrazolyl)borate Ligands
Charles G. Young; Simon Thomas; Robert W. Gable; Inorganic Chemistry 37 (1998) 1299–1306; doi:10.1021/ic970838w

data_4322701
_publ_section_title
;
 Halocarbonyltungsten(II) Complexes Containing Tripodal
 Tris(pyrazolyl)borate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1299
_journal_page_last               1306
_journal_paper_doi               10.1021/ic970838w
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C18 H22 B Br4 N7 O W'
_chemical_formula_weight         866.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     patt
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 128.61(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.245(4)
_cell_length_b                   19.077(4)
_cell_length_c                   15.639(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(1)
_cell_measurement_theta_max      13.8
_cell_measurement_theta_min      7.7
_cell_volume                     5186(2)
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  shelxl-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(1)
_diffrn_measurement_device       'Enraf-Nonius CAD4MachS diffractometer'
_diffrn_measurement_method       \w:2\q
_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    0.0515
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5274
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  160
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    10.644
_exptl_absorpt_correction_T_max  0.2714
_exptl_absorpt_correction_T_min  0.1900
_exptl_absorpt_correction_type   'gaussian integration (Sheldrick, 1976)'
_exptl_crystal_colour            'Dark Yellow'
_exptl_crystal_density_diffrn    2.220
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       needle
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.700
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.040
_refine_ls_goodness_of_fit_obs   1.115
_refine_ls_hydrogen_treatment    geom
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4565
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.043
_refine_ls_restrained_S_obs      1.115
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_obs          0.0515
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+31.6600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1207
_refine_ls_wR_factor_obs         0.1061
_reflns_number_observed          3179
_reflns_number_total             4569
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970838w_2.cif
_cod_data_source_block           '[L^Br^Br(MeCN)(CO)]'
_cod_depositor_comments
;
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^)+(0.0561P)^2^+31.6600P] 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^)+(0.0561P)^2^+31.6600P] 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        5186.0(17)
_cod_database_code               4322701