Synthesis, structure and properties of the mixed-ligand tungsten(II) complex [WBr2(CO)3(tmpymt)] (tmpymt = 1,4,6-trimethylpyrimidine-2-thione)
Falcomer, Viviane A.S.; Lemos, Sebastião S.; Politi, José R.S.; Casagrande, Gleison A.; Lang, Ernesto S.; Burrow, Robert A.; Inorganic Chemistry Communications 12 (2009) 580–582; doi:10.1016/j.inoche.2009.04.025

data_4350811
_publ_section_title
;
 Synthesis, structure and properties of the mixed-ligand tungsten(II)
 complex [WBr2(CO)3(tmpymt)] (tmpymt = 1,4,6-trimethylpyrimidine-2-thione)
;
_journal_issue                   6
_journal_name_full               'Inorganic Chemistry Communications'
_journal_page_first              580
_journal_page_last               582
_journal_paper_doi               10.1016/j.inoche.2009.04.025
_journal_volume                  12
_journal_year                    2009
_chemical_formula_moiety         'C10 H10 Br2 N2 O3 S W, C3 H6 O'
_chemical_formula_sum            'C13 H16 Br2 N2 O4 S W'
_chemical_formula_weight         640.01
_chemical_name_systematic
; 
 Dibromo-tricarbonyl-(1,4,6-trimethylpyrimidine-2-thione-\kN^3^,\kS)-
 tungsten(II) acetone solvate
;
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.7064(7)
_cell_length_b                   21.7064(7)
_cell_length_c                   7.3386(5)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.98
_cell_measurement_theta_min      2.65
_cell_volume                     3457.7(3)
_computing_cell_refinement       SAINT
_computing_data_collection       APEX2/BIS/COSMO
_computing_data_reduction        SAINT/XPREP/SADABS
_computing_molecular_graphics    'Crystal Impact Diamond 3'
_computing_publication_material  Vim
_computing_structure_refinement  XL
_computing_structure_solution    XS
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            103736
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    11.444
_exptl_absorpt_correction_T_max  0.2795
_exptl_absorpt_correction_T_min  0.0680
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 XPREP (Bruker, 2006) was used to perform the Gaussian numeric absorption 
 corrections; SADABS (Bruker, 2006) scaled the resulting data.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
 SQUEEZE (PLATON, A. Spek, 2007) was used to remove electron density from
 the disordered solvate molecules, corresponding to 32.6 electrons per 
 asymmetric unit, equivalent to one molecule of acetone (32 electrons).
;
_refine_diff_density_max         1.138
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         5079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0192P)^2^+5.7219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0503
_refine_ls_wR_factor_ref         0.0529
_reflns_number_gt                4203
_reflns_number_total             5079
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            Inorg6Chem-Commun-2009-12-580.cif
_cod_data_source_block           rb_sl_vf_wtmpymp_bob-sqz
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Tetragonal' was changed to
'tetragonal' in accordance with the built-in table derived from the
CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated
on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
;
_cod_original_sg_symbol_H-M      'P4/n  '
_cod_database_code               4350811