#------------------------------------------------------------------------------
#$Date: 2016-11-08 21:55:14 +0200 (Tue, 08 Nov 2016) $
#$Revision: 188190 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/06/7040674.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_7040674
loop_
_publ_author_name
'Poropudas, Merja J.'
'Rautiainen, J. Mikko'
'Oilunkaniemi, Raija'
'Laitinen, Risto S.'
_publ_section_title
;
 Synthesis, characterization, and ligand behaviour of a new ditelluroether
 (C10H7)Te(CH2)4Te(C10H7) and the concurrently formed ionic
 [(C10H7)Te(CH2)4]Br.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17206
_journal_page_last               17215
_journal_paper_doi               10.1039/c6dt02599d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C48 H44 Br2 Cu2 Te4'
_chemical_formula_weight         1418.13
_chemical_name_systematic
;
Bis{(mu-bromido)[mu-(1,4-bis(1-naphthyltelluro)butane]copper}
;
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-09-05 deposited with the CCDC.
2016-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                91.048(5)
_cell_angle_beta                 101.586(5)
_cell_angle_gamma                106.987(5)
_cell_formula_units_Z            1
_cell_length_a                   7.425(5)
_cell_length_b                   11.072(5)
_cell_length_c                   14.288(5)
_cell_measurement_reflns_used    3062
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.999
_cell_measurement_theta_min      2.938
_cell_volume                     1096.8(10)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Bruker, 2008)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Bruker Nonius Kappaccd'
_diffrn_measurement_method       'φ scans, and ω scans with κ offsets'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.914
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12420
_diffrn_reflns_point_group_measured_fraction_full 0.914
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.938
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.432
_exptl_absorpt_correction_T_max  0.9719
_exptl_absorpt_correction_T_min  0.7620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XPREP in SHELXTL (Sheldrick 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.147
_exptl_crystal_description       plate
_exptl_crystal_F_000             668
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.961
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.229
_refine_ls_extinction_coef       0.0035(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0275P)²+4.8143P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0852
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3062
_reflns_number_total             3619
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt02599d9.cif
_cod_data_source_block           cmpd3a
_cod_depositor_comments
'Adding full bibliography for 7040672--7040677.cif.'
_cod_database_code               7040674
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.496
_shelx_estimated_absorpt_t_max   0.948
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Cu1 Cu 0.43588(12) 0.56202(7) 0.58080(6) 0.0276(2) Uani 1 1 d . .
Te2 Te 0.58829(6) 0.21396(4) 0.45645(3) 0.02346(15) Uani 1 1 d . .
Te1 Te 0.26340(6) 0.46861(4) 0.71272(3) 0.02579(15) Uani 1 1 d . .
Br1 Br 0.76695(10) 0.55991(6) 0.57420(5) 0.02756(19) Uani 1 1 d . .
C1 C 0.1064(9) 0.2779(6) 0.6476(5) 0.0285(16) Uani 1 1 d . .
H1A H -0.0145 0.2479 0.6711 0.034 Uiso 1 1 calc R U
H1B H 0.0704 0.2815 0.5773 0.034 Uiso 1 1 calc R U
C2 C 0.2168(10) 0.1817(6) 0.6676(5) 0.0312(16) Uani 1 1 d . .
H2A H 0.1271 0.0961 0.6450 0.037 Uiso 1 1 calc R U
H2B H 0.2625 0.1834 0.7378 0.037 Uiso 1 1 calc R U
C3 C 0.3908(10) 0.2040(6) 0.6201(5) 0.0243(14) Uani 1 1 d . .
H3A H 0.4554 0.2963 0.6227 0.029 Uiso 1 1 calc R U
H3B H 0.4842 0.1651 0.6569 0.029 Uiso 1 1 calc R U
C4 C 0.3352(10) 0.1494(6) 0.5165(5) 0.0273(15) Uani 1 1 d . .
H4A H 0.2296 0.1787 0.4803 0.033 Uiso 1 1 calc R U
H4B H 0.2907 0.0556 0.5132 0.033 Uiso 1 1 calc R U
C10 C 0.4747(10) 0.4217(6) 0.8176(5) 0.0264(15) Uani 1 1 d . .
C11 C 0.6593(9) 0.4573(6) 0.8068(5) 0.0277(15) Uani 1 1 d . .
H11 H 0.6876 0.4967 0.7508 0.033 Uiso 1 1 calc R U
C12 C 0.8105(10) 0.4382(7) 0.8751(5) 0.0343(17) Uani 1 1 d . .
H12 H 0.9380 0.4625 0.8644 0.041 Uiso 1 1 calc R U
C13 C 0.7732(11) 0.3844(7) 0.9570(6) 0.0358(18) Uani 1 1 d . .
H13 H 0.8756 0.3725 1.0039 0.043 Uiso 1 1 calc R U
C14 C 0.5827(10) 0.3463(6) 0.9727(5) 0.0292(16) Uani 1 1 d . .
C15 C 0.5428(11) 0.2900(7) 1.0570(5) 0.0328(17) Uani 1 1 d . .
H15 H 0.6451 0.2790 1.1045 0.039 Uiso 1 1 calc R U
C16 C 0.3575(12) 0.2508(7) 1.0711(5) 0.0374(18) Uani 1 1 d . .
H16 H 0.3315 0.2131 1.1281 0.045 Uiso 1 1 calc R U
C17 C 0.2085(11) 0.2669(7) 1.0013(5) 0.0338(17) Uani 1 1 d . .
H17 H 0.0805 0.2390 1.0112 0.041 Uiso 1 1 calc R U
C18 C 0.2404(10) 0.3213(7) 0.9193(5) 0.0292(16) Uani 1 1 d . .
H18 H 0.1353 0.3311 0.8731 0.035 Uiso 1 1 calc R U
C19 C 0.4306(9) 0.3637(6) 0.9023(5) 0.0236(14) Uani 1 1 d . .
C20 C 0.4834(9) 0.0986(6) 0.3245(4) 0.0198(13) Uani 1 1 d . .
C21 C 0.2931(9) 0.0244(6) 0.2995(5) 0.0244(14) Uani 1 1 d . .
H21 H 0.2065 0.0280 0.3394 0.029 Uiso 1 1 calc R U
C22 C 0.2278(10) -0.0568(6) 0.2141(5) 0.0290(16) Uani 1 1 d . .
H22 H 0.0966 -0.1073 0.1971 0.035 Uiso 1 1 calc R U
C23 C 0.3493(10) -0.0643(6) 0.1555(5) 0.0262(15) Uani 1 1 d . .
H23 H 0.3023 -0.1200 0.0987 0.031 Uiso 1 1 calc R U
C24 C 0.5453(9) 0.0108(6) 0.1792(5) 0.0229(14) Uani 1 1 d . .
C25 C 0.6738(10) 0.0051(6) 0.1209(5) 0.0266(15) Uani 1 1 d . .
H25 H 0.6301 -0.0514 0.0646 0.032 Uiso 1 1 calc R U
C26 C 0.8616(10) 0.0801(7) 0.1441(5) 0.0325(17) Uani 1 1 d . .
H26 H 0.9472 0.0741 0.1043 0.039 Uiso 1 1 calc R U
C27 C 0.9291(10) 0.1656(7) 0.2258(5) 0.0306(16) Uani 1 1 d . .
H27 H 1.0587 0.2191 0.2400 0.037 Uiso 1 1 calc R U
C28 C 0.8089(9) 0.1719(6) 0.2849(5) 0.0259(15) Uani 1 1 d . .
H28 H 0.8571 0.2288 0.3410 0.031 Uiso 1 1 calc R U
C29 C 0.6144(9) 0.0959(6) 0.2646(5) 0.0193(13) Uani 1 1 d . .
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 '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'
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
Br1 Cu1 Br1 103.29(4) . 2_666
Br1 Cu1 Te1 123.69(4) . .
Br1 Cu1 Te1 106.26(5) 2_666 .
Br1 Cu1 Te2 107.76(3) . 2_666
Br1 Cu1 Te2 99.08(4) 2_666 2_666
Te1 Cu1 Te2 113.36(4) . 2_666
C20 Te2 C4 98.6(2) . .
C20 Te2 Cu1 106.89(16) . 2_666
C4 Te2 Cu1 98.05(18) . 2_666
C10 Te1 C1 98.0(3) . .
C10 Te1 Cu1 105.66(19) . .
C1 Te1 Cu1 100.75(19) . .
Cu1 Br1 Cu1 76.71(4) . 2_666
C2 C1 Te1 114.7(5) . .
C2 C1 H1A 108.6 . .
Te1 C1 H1A 108.6 . .
C2 C1 H1B 108.6 . .
Te1 C1 H1B 108.6 . .
H1A C1 H1B 107.6 . .
C1 C2 C3 114.5(6) . .
C1 C2 H2A 108.6 . .
C3 C2 H2A 108.6 . .
C1 C2 H2B 108.6 . .
C3 C2 H2B 108.6 . .
H2A C2 H2B 107.6 . .
C4 C3 C2 112.9(6) . .
C4 C3 H3A 109.0 . .
C2 C3 H3A 109.0 . .
C4 C3 H3B 109.0 . .
C2 C3 H3B 109.0 . .
H3A C3 H3B 107.8 . .
C3 C4 Te2 107.4(4) . .
C3 C4 H4A 110.2 . .
Te2 C4 H4A 110.2 . .
C3 C4 H4B 110.2 . .
Te2 C4 H4B 110.2 . .
H4A C4 H4B 108.5 . .
C11 C10 C19 119.3(7) . .
C11 C10 Te1 118.3(5) . .
C19 C10 Te1 122.2(5) . .
C10 C11 C12 122.6(7) . .
C10 C11 H11 118.7 . .
C12 C11 H11 118.7 . .
C13 C12 C11 119.5(7) . .
C13 C12 H12 120.3 . .
C11 C12 H12 120.3 . .
C12 C13 C14 120.5(7) . .
C12 C13 H13 119.7 . .
C14 C13 H13 119.7 . .
C19 C14 C15 119.7(7) . .
C19 C14 C13 119.5(7) . .
C15 C14 C13 120.8(7) . .
C16 C15 C14 120.7(7) . .
C16 C15 H15 119.7 . .
C14 C15 H15 119.7 . .
C15 C16 C17 119.4(7) . .
C15 C16 H16 120.3 . .
C17 C16 H16 120.3 . .
C18 C17 C16 122.0(7) . .
C18 C17 H17 119.0 . .
C16 C17 H17 119.0 . .
C17 C18 C19 120.3(7) . .
C17 C18 H18 119.8 . .
C19 C18 H18 119.8 . .
C14 C19 C18 118.0(6) . .
C14 C19 C10 118.7(6) . .
C18 C19 C10 123.4(6) . .
C21 C20 C29 120.8(6) . .
C21 C20 Te2 120.3(5) . .
C29 C20 Te2 118.8(4) . .
C20 C21 C22 119.7(6) . .
C20 C21 H21 120.1 . .
C22 C21 H21 120.1 . .
C23 C22 C21 121.4(6) . .
C23 C22 H22 119.3 . .
C21 C22 H22 119.3 . .
C22 C23 C24 120.2(6) . .
C22 C23 H23 119.9 . .
C24 C23 H23 119.9 . .
C25 C24 C23 121.6(6) . .
C25 C24 C29 118.9(6) . .
C23 C24 C29 119.5(6) . .
C26 C25 C24 120.7(6) . .
C26 C25 H25 119.6 . .
C24 C25 H25 119.6 . .
C25 C26 C27 120.9(6) . .
C25 C26 H26 119.6 . .
C27 C26 H26 119.6 . .
C28 C27 C26 119.9(6) . .
C28 C27 H27 120.1 . .
C26 C27 H27 120.1 . .
C27 C28 C29 121.5(6) . .
C27 C28 H28 119.3 . .
C29 C28 H28 119.3 . .
C28 C29 C20 123.5(6) . .
C28 C29 C24 118.1(6) . .
C20 C29 C24 118.3(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 Br1 2.486(2) .
Cu1 Br1 2.5215(13) 2_666
Cu1 Te1 2.5552(12) .
Cu1 Te2 2.5957(14) 2_666
Te2 C20 2.129(6) .
Te2 C4 2.160(6) .
Te2 Cu1 2.5957(14) 2_666
Te1 C10 2.130(7) .
Te1 C1 2.177(7) .
Br1 Cu1 2.5215(13) 2_666
C1 C2 1.522(10) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 C3 1.537(9) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.517(9) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C10 C11 1.352(9) .
C10 C19 1.432(9) .
C11 C12 1.401(10) .
C11 H11 0.9500 .
C12 C13 1.363(11) .
C12 H12 0.9500 .
C13 C14 1.418(10) .
C13 H13 0.9500 .
C14 C19 1.415(10) .
C14 C15 1.411(10) .
C15 C16 1.374(11) .
C15 H15 0.9500 .
C16 C17 1.388(11) .
C16 H16 0.9500 .
C17 C18 1.358(10) .
C17 H17 0.9500 .
C18 C19 1.424(9) .
C18 H18 0.9500 .
C20 C21 1.381(9) .
C20 C29 1.425(9) .
C21 C22 1.414(9) .
C21 H21 0.9500 .
C22 C23 1.366(9) .
C22 H22 0.9500 .
C23 C24 1.418(9) .
C23 H23 0.9500 .
C24 C25 1.400(9) .
C24 C29 1.437(9) .
C25 C26 1.368(10) .
C25 H25 0.9500 .
C26 C27 1.398(10) .
C26 H26 0.9500 .
C27 C28 1.360(9) .
C27 H27 0.9500 .
C28 C29 1.411(9) .
C28 H28 0.9500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
Te1 C1 C2 C3 -68.1(7)
C1 C2 C3 C4 -83.2(7)
C2 C3 C4 Te2 171.6(4)
C19 C10 C11 C12 0.8(10)
Te1 C10 C11 C12 175.7(5)
C10 C11 C12 C13 -1.5(11)
C11 C12 C13 C14 0.9(11)
C12 C13 C14 C19 0.4(10)
C12 C13 C14 C15 179.7(7)
C19 C14 C15 C16 0.6(10)
C13 C14 C15 C16 -178.7(7)
C14 C15 C16 C17 0.1(11)
C15 C16 C17 C18 -0.5(11)
C16 C17 C18 C19 0.2(11)
C15 C14 C19 C18 -0.9(9)
C13 C14 C19 C18 178.4(6)
C15 C14 C19 C10 179.6(6)
C13 C14 C19 C10 -1.1(9)
C17 C18 C19 C14 0.5(10)
C17 C18 C19 C10 180.0(6)
C11 C10 C19 C14 0.5(10)
Te1 C10 C19 C14 -174.2(5)
C11 C10 C19 C18 -179.0(6)
Te1 C10 C19 C18 6.3(9)
C29 C20 C21 C22 1.0(9)
Te2 C20 C21 C22 -176.6(5)
C20 C21 C22 C23 0.3(10)
C21 C22 C23 C24 -0.4(10)
C22 C23 C24 C25 179.8(6)
C22 C23 C24 C29 -0.8(9)
C23 C24 C25 C26 178.8(6)
C29 C24 C25 C26 -0.6(9)
C24 C25 C26 C27 -1.0(10)
C25 C26 C27 C28 2.0(11)
C26 C27 C28 C29 -1.5(10)
C27 C28 C29 C20 179.6(6)
C27 C28 C29 C24 0.0(9)
C21 C20 C29 C28 178.2(6)
Te2 C20 C29 C28 -4.1(8)
C21 C20 C29 C24 -2.2(9)
Te2 C20 C29 C24 175.5(4)
C25 C24 C29 C28 1.1(9)
C23 C24 C29 C28 -178.3(6)
C25 C24 C29 C20 -178.5(6)
C23 C24 C29 C20 2.0(9)
