The heteroscorpionate ligand 2,2-bis(3,5-dimethylpyrazol-1-yl)-1,1-diphenylethanol and an easy preparation of its tungsten complex
Böhme, Uwe; Schwarzer, Anke; Günther, Betty; Acta Crystallographica Section C 75 (2019) –; doi:10.1107/S2053229619008362

data_2021687
_publ_section_title
;
 The heteroscorpionate ligand
 2,2-bis(3,5-dimethylpyrazol-1-yl)-1,1-diphenylethanol and an easy
 preparation of its tungsten complex
;
_journal_coeditor_code           FN3307
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229619008362
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[W (C24 H25 N4 O1) Cl O2], C4 H8 O'
_chemical_formula_moiety         'C24 H25 Cl N4 O3 W, C4 H8 O'
_chemical_formula_sum            'C28 H33 Cl N4 O4 W'
_chemical_formula_weight         708.88
_chemical_name_systematic
'<i>cis</i>-[2,2-Bis(3,5-dimethylpyrazolyl)-1,1-diphenylethanolato]chloridodioxidotungsten(VI) tetrahydrofuran monosolvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 93.222(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.3157(6)
_cell_length_b                   8.4063(3)
_cell_length_c                   17.4678(10)
_cell_measurement_reflns_used    12354
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.83
_cell_measurement_theta_min      2.69
_cell_volume                     1365.75(13)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2009)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2009)
;
_computing_data_reduction
;
X-RED (Stoe & Cie, 2009)
;
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 2012)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      153
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12354
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         3.111
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.368
_exptl_absorpt_correction_T_max  0.6391
_exptl_absorpt_correction_T_min  0.3906
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-RED; Stoe & Cie, 2009)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_description       Prism
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.937
_refine_diff_density_min         -1.065
_refine_ls_abs_structure_details
;
Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.489(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5165
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0148P)^2^+4.1365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0519
_refine_ls_wR_factor_ref         0.0545
_reflns_number_gt                4924
_reflns_number_total             5165
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fn3307sup1.cif
_cod_data_source_block           2
_cod_database_code               2021687
_shelx_estimated_absorpt_t_min   0.408
_shelx_estimated_absorpt_t_max   0.669
_shelx_hkl_checksum              41457
_shelx_res_checksum              54599