#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:34:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179452 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/49/4334987.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_4334987
loop_
_publ_author_name
'Erik V. Johnstone'
'Daniel J. Grant'
'Frederic Poineau'
'Laura Fox'
'Paul M. Forster'
'Longzou Ma'
'Laura Gagliardi'
'Kenneth R. Czerwinski'
'Alfred P. Sattelberger'
_publ_section_title
;
 A Trigonal-Prismatic Hexanuclear Technetium(II) Bromide Cluster:
 Solid-State Synthesis and Crystallographic and Electronic Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5660
_journal_page_last               5662
_journal_paper_doi               10.1021/ic400967k
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'Br25 Na Tc12'
_chemical_formula_weight         3196.74
_chemical_name_systematic
; 
 ? 
;
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.6700(10)
_cell_angle_beta                 73.7290(10)
_cell_angle_gamma                87.4880(10)
_cell_formula_units_Z            1
_cell_length_a                   9.5173(5)
_cell_length_b                   10.5233(6)
_cell_length_c                   11.1412(6)
_cell_measurement_temperature    100(2)
_cell_volume                     1064.51(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17149
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    27.238
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.3078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Area-Detector Absorption Correction; Siemens Industrial Automation, Inc. 
Madison, WI, 1996
;
_exptl_crystal_density_diffrn    4.987
_exptl_crystal_F_000             1402
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.769
_refine_diff_density_min         -1.958
_refine_diff_density_rms         0.366
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         6456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0252
_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)+(0.0435P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0751
_reflns_number_gt                5858
_reflns_number_total             6456
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400967k_si_002.cif
_cod_data_source_block           fp_tcbr2_a_0m_a
_cod_database_code               4334987
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Tc01 Tc 0.17301(3) 0.74663(3) 0.88058(3) 0.00624(7) Uani 1 1 d .
Tc02 Tc 0.25022(3) 0.88430(3) 0.71803(3) 0.00628(7) Uani 1 1 d .
Tc03 Tc -0.07121(3) 0.72589(3) 0.80848(3) 0.00663(7) Uani 1 1 d .
Tc04 Tc 0.15716(3) 0.56797(3) 0.73203(3) 0.00668(7) Uani 1 1 d .
Tc05 Tc 0.23713(4) 0.70343(3) 0.56649(3) 0.00668(7) Uani 1 1 d .
Tc06 Tc 0.00902(3) 0.86100(3) 0.64266(3) 0.00665(7) Uani 1 1 d .
Br2 Br 0.05423(4) 1.04827(4) 0.74129(4) 0.00801(8) Uani 1 1 d .
Br4 Br 0.03125(4) 0.72190(4) 0.47240(4) 0.00891(8) Uani 1 1 d .
Br11 Br 0.35962(4) 0.57317(4) 0.83252(4) 0.00872(8) Uani 1 1 d .
Br9 Br -0.09359(4) 0.52617(4) 0.71851(4) 0.00908(8) Uani 1 1 d .
Br13 Br 0.0000 0.5000 1.0000 0.01321(12) Uani 1 2 d S
Br1 Br 0.40823(4) 1.04489(4) 0.76555(4) 0.01061(9) Uani 1 1 d .
Br3 Br -0.20873(4) 0.97516(4) 0.58873(4) 0.00961(8) Uani 1 1 d .
Br6 Br 0.46945(4) 0.78402(4) 0.58488(4) 0.00941(8) Uani 1 1 d .
Br7 Br -0.06645(4) 0.84238(4) 0.98676(4) 0.00821(8) Uani 1 1 d .
Br10 Br 0.23046(5) 0.34758(4) 0.68187(4) 0.01204(9) Uani 1 1 d .
Br12 Br 0.26687(4) 0.79188(4) 1.06175(4) 0.01132(9) Uani 1 1 d .
Br8 Br -0.34360(4) 0.74176(4) 0.88365(5) 0.01376(9) Uani 1 1 d .
Br5 Br 0.37453(5) 0.58716(5) 0.38957(4) 0.01496(10) Uani 1 1 d .
Na1 Na 0.5000 1.0000 1.0000 0.0239(6) Uani 1 2 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Na Na 0.0362 0.0249 '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
Tc02 Tc01 Br7 101.612(18) . .
Tc02 Tc01 Br11 101.240(19) . .
Br7 Tc01 Br11 155.87(2) . .
Tc02 Tc01 Br12 112.027(19) . .
Br7 Tc01 Br12 88.925(17) . .
Br11 Tc01 Br12 89.652(17) . .
Tc02 Tc01 Tc04 90.601(17) . .
Br7 Tc01 Tc04 114.481(16) . .
Br11 Tc01 Tc04 57.599(13) . .
Br12 Tc01 Tc04 143.977(18) . .
Tc02 Tc01 Tc03 87.976(16) . .
Br7 Tc01 Tc03 56.613(14) . .
Br11 Tc01 Tc03 116.767(17) . .
Br12 Tc01 Tc03 143.735(18) . .
Tc04 Tc01 Tc03 59.921(12) . .
Tc01 Tc02 Br2 104.039(19) . .
Tc01 Tc02 Br6 105.182(19) . .
Br2 Tc02 Br6 149.54(2) . .
Tc01 Tc02 Br1 109.822(19) . .
Br2 Tc02 Br1 88.093(17) . .
Br6 Tc02 Br1 89.995(17) . .
Tc01 Tc02 Tc06 92.287(16) . .
Br2 Tc02 Tc06 57.101(13) . .
Br6 Tc02 Tc06 113.118(17) . .
Br1 Tc02 Tc06 142.934(18) . .
Tc01 Tc02 Tc05 89.661(16) . .
Br2 Tc02 Tc05 115.242(17) . .
Br6 Tc02 Tc05 56.812(13) . .
Br1 Tc02 Tc05 145.520(18) . .
Tc06 Tc02 Tc05 59.417(12) . .
Tc06 Tc03 Br7 104.993(19) . .
Tc06 Tc03 Br9 103.077(19) . .
Br7 Tc03 Br9 151.27(2) . .
Tc06 Tc03 Br8 109.645(19) . .
Br7 Tc03 Br8 86.920(17) . .
Br9 Tc03 Br8 89.400(17) . .
Tc06 Tc03 Tc04 91.496(16) . .
Br7 Tc03 Tc04 115.152(17) . .
Br9 Tc03 Tc04 57.809(13) . .
Br8 Tc03 Tc04 144.824(19) . .
Tc06 Tc03 Tc01 91.924(16) . .
Br7 Tc03 Tc01 57.462(13) . .
Br9 Tc03 Tc01 115.788(16) . .
Br8 Tc03 Tc01 142.589(19) . .
Tc04 Tc03 Tc01 59.772(12) . .
Tc05 Tc04 Br10 110.39(2) . .
Tc05 Tc04 Br11 100.521(18) . .
Br10 Tc04 Br11 89.770(17) . .
Tc05 Tc04 Br9 101.283(19) . .
Br10 Tc04 Br9 89.270(17) . .
Br11 Tc04 Br9 157.06(2) . .
Tc05 Tc04 Tc01 90.321(16) . .
Br10 Tc04 Tc01 144.500(19) . .
Br11 Tc04 Tc01 57.380(13) . .
Br9 Tc04 Tc01 115.406(16) . .
Tc05 Tc04 Tc03 88.386(16) . .
Br10 Tc04 Tc03 144.544(18) . .
Br11 Tc04 Tc03 116.931(17) . .
Br9 Tc04 Tc03 56.876(13) . .
Tc01 Tc04 Tc03 60.307(12) . .
Tc05 Tc04 Br13 153.147(17) . .
Br10 Tc04 Br13 96.467(16) . .
Br11 Tc04 Br13 78.830(14) . .
Br9 Tc04 Br13 78.511(14) . .
Tc01 Tc04 Br13 66.466(11) . .
Tc03 Tc04 Br13 68.804(11) . .
Tc04 Tc05 Br5 109.32(2) . .
Tc04 Tc05 Br4 102.814(18) . .
Br5 Tc05 Br4 88.299(18) . .
Tc04 Tc05 Br6 105.534(19) . .
Br5 Tc05 Br6 89.792(17) . .
Br4 Tc05 Br6 150.55(2) . .
Tc04 Tc05 Tc06 91.624(16) . .
Br5 Tc05 Tc06 143.697(19) . .
Br4 Tc05 Tc06 57.587(14) . .
Br6 Tc05 Tc06 113.388(17) . .
Tc04 Tc05 Tc02 89.412(17) . .
Br5 Tc05 Tc02 145.460(18) . .
Br4 Tc05 Tc02 116.321(17) . .
Br6 Tc05 Tc02 56.660(13) . .
Tc06 Tc05 Tc02 59.854(12) . .
Tc03 Tc06 Br2 100.466(19) . .
Tc03 Tc06 Br4 101.042(19) . .
Br2 Tc06 Br4 157.18(2) . .
Tc03 Tc06 Br3 108.511(18) . .
Br2 Tc06 Br3 90.334(17) . .
Br4 Tc06 Br3 90.014(17) . .
Tc03 Tc06 Tc05 88.495(16) . .
Br2 Tc06 Tc05 116.356(17) . .
Br4 Tc06 Tc05 56.875(13) . .
Br3 Tc06 Tc05 145.651(19) . .
Tc03 Tc06 Tc02 87.790(16) . .
Br2 Tc06 Tc02 56.930(13) . .
Br4 Tc06 Tc02 116.481(16) . .
Br3 Tc06 Tc02 146.118(18) . .
Tc05 Tc06 Tc02 60.729(12) . .
Tc02 Br2 Tc06 65.970(15) . .
Tc05 Br4 Tc06 65.538(14) . .
Tc01 Br11 Tc04 65.021(14) . .
Tc03 Br9 Tc04 65.315(14) . .
Tc04 Br13 Tc04 179.999(12) . 2_567
Tc02 Br1 Na1 119.227(18) . .
Tc02 Br6 Tc05 66.527(15) . .
Tc03 Br7 Tc01 65.926(14) . .
Tc01 Br12 Na1 115.240(18) . .
Tc03 Br8 Na1 119.971(17) . 1_455
Br1 Na1 Br1 180.0 2_677 .
Br1 Na1 Br12 97.999(12) 2_677 .
Br1 Na1 Br12 82.002(12) . .
Br1 Na1 Br12 82.001(12) 2_677 2_677
Br1 Na1 Br12 97.998(12) . 2_677
Br12 Na1 Br12 180.000(16) . 2_677
Br1 Na1 Br8 84.772(12) 2_677 2_577
Br1 Na1 Br8 95.228(12) . 2_577
Br12 Na1 Br8 107.912(12) . 2_577
Br12 Na1 Br8 72.087(11) 2_677 2_577
Br1 Na1 Br8 95.228(12) 2_677 1_655
Br1 Na1 Br8 84.772(12) . 1_655
Br12 Na1 Br8 72.088(11) . 1_655
Br12 Na1 Br8 107.913(11) 2_677 1_655
Br8 Na1 Br8 180.0 2_577 1_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tc01 Tc02 2.1651(5) .
Tc01 Br7 2.4819(5) .
Tc01 Br11 2.4841(5) .
Tc01 Br12 2.5216(5) .
Tc01 Tc04 2.6735(5) .
Tc01 Tc03 2.6879(5) .
Tc02 Br2 2.4636(5) .
Tc02 Br6 2.4669(5) .
Tc02 Br1 2.5028(5) .
Tc02 Tc06 2.6850(5) .
Tc02 Tc05 2.7085(5) .
Tc03 Tc06 2.1779(5) .
Tc03 Br7 2.4581(5) .
Tc03 Br9 2.4679(5) .
Tc03 Br8 2.4953(5) .
Tc03 Tc04 2.6775(5) .
Tc04 Tc05 2.1776(5) .
Tc04 Br10 2.4704(5) .
Tc04 Br11 2.4902(5) .
Tc04 Br9 2.4938(5) .
Tc04 Br13 2.9635(4) .
Tc05 Br5 2.4575(5) .
Tc05 Br4 2.4594(5) .
Tc05 Br6 2.4712(5) .
Tc05 Tc06 2.6730(5) .
Tc06 Br2 2.4684(5) .
Tc06 Br4 2.4791(5) .
Tc06 Br3 2.5336(5) .
Br13 Tc04 2.9635(4) 2_567
Br1 Na1 2.9630(5) .
Br12 Na1 3.0710(4) .
Br8 Na1 3.2591(5) 1_455
Na1 Br1 2.9630(5) 2_677
Na1 Br12 3.0710(4) 2_677
Na1 Br8 3.2591(5) 2_577
Na1 Br8 3.2591(5) 1_655
