Synthesis, structure, and first-principles calculations of [TcBr2(PMe3)4] and [Tc2Br4(PMe3)4] complexes
Poineau, Frederic; Weck, Philippe F.; Forster, Paul M.; Sattelberger, Alfred P.; Czerwinski, Kenneth R.; Dalton Transactions  (2009) 10338–10342; doi:10.1039/b915968a

data_7002848
_publ_section_title
;
 Synthesis, structure, and first-principles calculations of
 [TcBr2(PMe3)4] and [Tc2Br4(PMe3)4] complexes
;
_journal_issue                   46
_journal_name_full               'Dalton Transactions'
_journal_page_first              10338
_journal_page_last               10342
_journal_paper_doi               10.1039/b915968a
_journal_year                    2009
_chemical_formula_sum            'C6 H18 Br2 P2 Tc'
_chemical_formula_weight         409.96
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.1040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.0903(19)
_cell_length_b                   9.3365(10)
_cell_length_c                   17.232(3)
_cell_measurement_temperature    150(2)
_cell_volume                     2635.6(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18170
_diffrn_reflns_theta_full        28.52
_diffrn_reflns_theta_max         28.52
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    7.352
_exptl_absorpt_correction_T_max  .7457
_exptl_absorpt_correction_T_min  0.6428
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.786
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         3335
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+8.7069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0638
_reflns_number_gt                2999
_reflns_number_total             3335
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b915968a.txt
_cod_data_source_block           Tc2Br4(PMe3)4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2635.5(6)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7002848