#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:44:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179732 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/28/7002848.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7002848
loop_
_publ_author_name
'Poineau, Frederic'
'Weck, Philippe F.'
'Forster, Paul M.'
'Sattelberger, Alfred P.'
'Czerwinski, Kenneth R.'
_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/[σ²(Fo²)+(0.0309P)²+8.7069P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tc1 Tc 0.5000 0.32584(3) 0.2500 0.01635(8) Uani 1 2 d S . .
Tc2 Tc 0.5000 0.09753(3) 0.2500 0.01558(8) Uani 1 2 d S . .
Br1 Br 0.38767(2) 0.43740(4) 0.12021(2) 0.02877(9) Uani 1 1 d . . .
Br2 Br 0.58275(2) -0.01354(4) 0.17930(2) 0.02639(8) Uani 1 1 d . . .
P1 P 0.58735(5) 0.38119(9) 0.17780(5) 0.02441(17) Uani 1 1 d . . .
P2 P 0.38290(5) 0.04109(9) 0.11569(5) 0.02217(16) Uani 1 1 d . . .
C1 C 0.5947(3) 0.5765(4) 0.1741(3) 0.0368(8) Uani 1 1 d . . .
H1A H 0.5409 0.6171 0.1490 0.055 Uiso 1 1 calc R . .
H1B H 0.6232 0.6019 0.1401 0.055 Uiso 1 1 calc R . .
H1C H 0.6239 0.6129 0.2312 0.055 Uiso 1 1 calc R . .
C2 C 0.6940(2) 0.3280(4) 0.2257(3) 0.0388(9) Uani 1 1 d . . .
H2A H 0.7176 0.3497 0.2859 0.058 Uiso 1 1 calc R . .
H2B H 0.7228 0.3792 0.1988 0.058 Uiso 1 1 calc R . .
H2C H 0.6980 0.2269 0.2179 0.058 Uiso 1 1 calc R . .
C3 C 0.5547(3) 0.3319(4) 0.0658(2) 0.0363(8) Uani 1 1 d . . .
H3A H 0.4982 0.3562 0.0340 0.054 Uiso 1 1 calc R . .
H3B H 0.5618 0.2307 0.0617 0.054 Uiso 1 1 calc R . .
H3C H 0.5870 0.3829 0.0427 0.054 Uiso 1 1 calc R . .
C4 C 0.2816(2) 0.0947(4) 0.1024(2) 0.0318(7) Uani 1 1 d . . .
H4A H 0.2755 0.0738 0.1539 0.048 Uiso 1 1 calc R . .
H4B H 0.2412 0.0429 0.0554 0.048 Uiso 1 1 calc R . .
H4C H 0.2746 0.1956 0.0909 0.048 Uiso 1 1 calc R . .
C5 C 0.3821(2) 0.0897(4) 0.0131(2) 0.0337(8) Uani 1 1 d . . .
H5A H 0.4337 0.0654 0.0131 0.051 Uiso 1 1 calc R . .
H5B H 0.3729 0.1908 0.0040 0.051 Uiso 1 1 calc R . .
H5C H 0.3393 0.0384 -0.0320 0.051 Uiso 1 1 calc R . .
C6 C 0.3739(2) -0.1538(4) 0.1079(2) 0.0363(8) Uani 1 1 d . . .
H6A H 0.3736 -0.1917 0.1595 0.054 Uiso 1 1 calc R . .
H6B H 0.4194 -0.1928 0.1000 0.054 Uiso 1 1 calc R . .
H6C H 0.3240 -0.1794 0.0599 0.054 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tc Tc -1.4390 0.7593 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Tc2 Tc1 P1 102.20(2) . . ?
Tc2 Tc1 P1 102.20(2) . 2_655 ?
P1 Tc1 P1 155.60(4) . 2_655 ?
Tc2 Tc1 Br1 114.393(11) . 2_655 ?
P1 Tc1 Br1 84.98(2) . 2_655 ?
P1 Tc1 Br1 85.01(2) 2_655 2_655 ?
Tc2 Tc1 Br1 114.393(11) . . ?
P1 Tc1 Br1 85.01(2) . . ?
P1 Tc1 Br1 84.98(2) 2_655 . ?
Br1 Tc1 Br1 131.21(2) 2_655 . ?
Tc1 Tc2 P2 102.46(2) . . ?
Tc1 Tc2 P2 102.46(2) . 2_655 ?
P2 Tc2 P2 155.07(4) . 2_655 ?
Tc1 Tc2 Br2 114.305(11) . . ?
P2 Tc2 Br2 84.68(2) . . ?
P2 Tc2 Br2 85.12(2) 2_655 . ?
Tc1 Tc2 Br2 114.305(11) . 2_655 ?
P2 Tc2 Br2 85.12(2) . 2_655 ?
P2 Tc2 Br2 84.68(2) 2_655 2_655 ?
Br2 Tc2 Br2 131.39(2) . 2_655 ?
C2 P1 C3 102.5(2) . . ?
C2 P1 C1 102.08(18) . . ?
C3 P1 C1 102.12(18) . . ?
C2 P1 Tc1 120.12(13) . . ?
C3 P1 Tc1 119.79(13) . . ?
C1 P1 Tc1 107.49(13) . . ?
C4 P2 C5 102.54(17) . . ?
C4 P2 C6 102.19(18) . . ?
C5 P2 C6 102.29(18) . . ?
C4 P2 Tc2 118.86(12) . . ?
C5 P2 Tc2 120.88(12) . . ?
C6 P2 Tc2 107.42(13) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tc1 Tc2 2.1316(5) . ?
Tc1 P1 2.4454(8) . ?
Tc1 P1 2.4454(8) 2_655 ?
Tc1 Br1 2.5218(4) 2_655 ?
Tc1 Br1 2.5218(4) . ?
Tc2 P2 2.4415(8) . ?
Tc2 P2 2.4415(8) 2_655 ?
Tc2 Br2 2.5196(4) . ?
Tc2 Br2 2.5196(4) 2_655 ?
P1 C2 1.816(4) . ?
P1 C3 1.822(4) . ?
P1 C1 1.832(4) . ?
P2 C4 1.819(3) . ?
P2 C5 1.819(3) . ?
P2 C6 1.827(4) . ?
