Mono- and di-nuclear tris(pyrazolyl)borato-oxo-tungsten(V) complexes with phenolate ligands: syntheses and structures, and magnetic, electrochemical and UV/Vis/NIR spectroscopic properties
Keira M. Stobie; Zöe R. Bell; Thomas W. Munhoven; John P. Maher; Jon A. McCleverty; Michael D. Ward; Eric J. L. McInnes; Federico Totti; Dante Gatteschi; Dalton Trans.  (2003) 36–45; doi:10.1039/b208397c

data_7012195
_publ_section_title
;
 Mono- and di-nuclear tris(pyrazolyl)borato-oxo-tungsten(V) complexes
 with phenolate ligands: syntheses and structures, and magnetic,
 electrochemical and UV/Vis/NIR spectroscopic properties
;
_journal_issue                   1
_journal_name_full               'Dalton Trans.'
_journal_page_first              36
_journal_page_last               45
_journal_paper_doi               10.1039/b208397c
_journal_year                    2003
_chemical_formula_sum            'C21 H27 B Cl N6 O2 W'
_chemical_formula_weight         625.60
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.39(3)
_cell_angle_beta                 76.986(19)
_cell_angle_gamma                66.99(2)
_cell_formula_units_Z            2
_cell_length_a                   10.429(4)
_cell_length_b                   11.283(4)
_cell_length_c                   11.437(5)
_cell_measurement_temperature    173(2)
_cell_volume                     1206.4(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens SMART Area Detector'
_diffrn_measurement_method
'\w rotation with narrow frames (0.3 degrees)'
_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  0.1370
_diffrn_reflns_av_sigmaI/netI    0.1062
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8793
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    4.928
_exptl_absorpt_correction_T_max  0.60
_exptl_absorpt_correction_T_min  0.09
_exptl_absorpt_correction_type   'Empirical, pseudo-azimuthal scan (SADABS)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             614
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.327
_refine_diff_density_min         -2.615
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         3355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1316
_reflns_number_gt                2903
_reflns_number_total             3355
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b208397c.txt
_cod_data_source_block           complex1
_cod_original_cell_volume        1206.5(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7012195