#------------------------------------------------------------------------------
#$Date: 2016-11-08 21:55:14 +0200 (Tue, 08 Nov 2016) $
#$Revision: 188190 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/06/7040675.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_7040675
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      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-06-27 deposited with the CCDC.
2016-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.32(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.679(3)
_cell_length_b                   12.479(3)
_cell_length_c                   11.389(2)
_cell_measurement_reflns_used    3225
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.999
_cell_measurement_theta_min      2.851
_cell_volume                     2214.8(8)
_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      120(2)
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.950
_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  0.0864
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.925
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            23226
_diffrn_reflns_point_group_measured_fraction_full 0.925
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.851
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.380
_exptl_absorpt_correction_T_max  0.9904
_exptl_absorpt_correction_T_min  0.8154
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XPREP in SHELXTL (Sheldrick 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.126
_exptl_crystal_description       plate
_exptl_crystal_F_000             1336
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.010
_refine_diff_density_max         4.395
_refine_diff_density_min         -1.383
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0606
_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)+(0.0167P)²+81.4102P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1283
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3225
_reflns_number_total             3706
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt02599d9.cif
_cod_data_source_block           cmpd3b
_cod_depositor_comments
'Adding full bibliography for 7040672--7040677.cif.'
_cod_original_cell_volume        2214.9(8)
_cod_database_code               7040675
_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   0.499
_shelx_estimated_absorpt_t_max   0.948
_shelxl_version_number           2013-4
_solvent_exptl_crystal_recrystallization_method dichloromethane
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Te1 Te 0.41573(5) 0.76713(5) 0.41515(6) 0.0202(2) Uani 1 1 d . .
Te2 Te 0.65117(5) 0.53498(6) 0.73650(6) 0.0221(2) Uani 1 1 d . .
Br1 Br 0.42315(7) 0.48480(8) 0.63086(9) 0.0215(3) Uani 1 1 d . .
Cu1 Cu 0.43222(9) 0.56464(10) 0.43675(12) 0.0216(3) Uani 1 1 d . .
C1 C 0.4850(7) 0.8539(9) 0.5631(9) 0.022(2) Uani 1 1 d . .
H1A H 0.4653 0.9293 0.5605 0.026 Uiso 1 1 calc R U
H1B H 0.4701 0.8222 0.6379 0.026 Uiso 1 1 calc R U
C2 C 0.5813(7) 0.8525(9) 0.5639(10) 0.025(3) Uani 1 1 d . .
H2A H 0.6063 0.9034 0.6249 0.030 Uiso 1 1 calc R U
H2B H 0.5956 0.8790 0.4865 0.030 Uiso 1 1 calc R U
C3 C 0.6246(8) 0.7427(9) 0.5876(11) 0.027(3) Uani 1 1 d . .
H3A H 0.6065 0.6939 0.5209 0.033 Uiso 1 1 calc R U
H3B H 0.6876 0.7514 0.5923 0.033 Uiso 1 1 calc R U
C4 C 0.6014(8) 0.6932(9) 0.7013(10) 0.025(3) Uani 1 1 d . .
H4A H 0.5381 0.6906 0.6984 0.031 Uiso 1 1 calc R U
H4B H 0.6230 0.7404 0.7679 0.031 Uiso 1 1 calc R U
C10 C 0.2971(7) 0.8035(8) 0.4816(9) 0.017(2) Uani 1 1 d . .
C11 C 0.2768(7) 0.7509(9) 0.5773(10) 0.025(3) Uani 1 1 d . .
H11 H 0.3119 0.6927 0.6069 0.030 Uiso 1 1 calc R U
C12 C 0.2048(7) 0.7791(9) 0.6361(10) 0.025(2) Uani 1 1 d . .
H12 H 0.1927 0.7407 0.7044 0.029 Uiso 1 1 calc R U
C13 C 0.1532(7) 0.8608(9) 0.5945(10) 0.025(3) Uani 1 1 d . .
H13 H 0.1048 0.8797 0.6335 0.029 Uiso 1 1 calc R U
C14 C 0.1715(7) 0.9187(8) 0.4919(9) 0.016(2) Uani 1 1 d . .
C15 C 0.1195(7) 1.0061(9) 0.4472(10) 0.024(2) Uani 1 1 d . .
H15 H 0.0721 1.0278 0.4869 0.029 Uiso 1 1 calc R U
C16 C 0.1372(7) 1.0595(9) 0.3470(10) 0.026(3) Uani 1 1 d . .
H16 H 0.1017 1.1172 0.3172 0.031 Uiso 1 1 calc R U
C17 C 0.2073(7) 1.0291(8) 0.2891(10) 0.023(2) Uani 1 1 d . .
H17 H 0.2187 1.0664 0.2198 0.027 Uiso 1 1 calc R U
C18 C 0.2599(7) 0.9467(8) 0.3298(9) 0.020(2) Uani 1 1 d . .
H18 H 0.3074 0.9276 0.2890 0.024 Uiso 1 1 calc R U
C19 C 0.2437(7) 0.8895(7) 0.4337(9) 0.014(2) Uani 1 1 d . .
C20 C 0.7774(7) 0.5582(9) 0.6950(10) 0.024(2) Uani 1 1 d . .
C21 C 0.8053(8) 0.4953(10) 0.6092(11) 0.031(3) Uani 1 1 d . .
H21 H 0.7652 0.4526 0.5611 0.038 Uiso 1 1 calc R U
C22 C 0.8919(10) 0.4925(13) 0.5909(13) 0.053(4) Uani 1 1 d . .
H22 H 0.9104 0.4476 0.5313 0.063 Uiso 1 1 calc R U
C23 C 0.9506(9) 0.5549(15) 0.6593(14) 0.057(5) Uani 1 1 d . .
H23 H 1.0095 0.5512 0.6473 0.068 Uiso 1 1 calc R U
C24 C 0.9254(9) 0.6228(12) 0.7448(13) 0.043(4) Uani 1 1 d . .
C25 C 0.9850(10) 0.6926(15) 0.8203(18) 0.065(6) Uani 1 1 d . .
H25 H 1.0440 0.6943 0.8084 0.077 Uiso 1 1 calc R U
C26 C 0.9567(12) 0.7539(13) 0.9060(19) 0.067(6) Uani 1 1 d . .
H26 H 0.9964 0.7966 0.9546 0.081 Uiso 1 1 calc R U
C27 C 0.8721(9) 0.7555(10) 0.9238(15) 0.051(5) Uani 1 1 d . .
H27 H 0.8539 0.8000 0.9840 0.061 Uiso 1 1 calc R U
C28 C 0.8129(9) 0.6944(10) 0.8567(12) 0.036(3) Uani 1 1 d . .
H28 H 0.7544 0.6977 0.8712 0.043 Uiso 1 1 calc R U
C29 C 0.8373(7) 0.6247(9) 0.7637(11) 0.028(3) 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
C10 Te1 C1 90.0(4) . .
C10 Te1 Cu1 105.1(3) . .
C1 Te1 Cu1 112.3(3) . .
C20 Te2 C4 99.4(4) . .
C20 Te2 Cu1 107.8(3) . 3_666
C4 Te2 Cu1 99.1(3) . 3_666
Cu1 Br1 Cu1 71.52(6) . 3_666
Br1 Cu1 Te1 118.43(6) . .
Br1 Cu1 Br1 108.48(6) . 3_666
Te1 Cu1 Br1 107.15(6) . 3_666
Br1 Cu1 Te2 115.02(6) . 3_666
Te1 Cu1 Te2 111.62(6) . 3_666
Br1 Cu1 Te2 92.60(6) 3_666 3_666
Br1 Cu1 Cu1 55.93(5) . 3_666
Te1 Cu1 Cu1 131.00(8) . 3_666
Br1 Cu1 Cu1 52.55(5) 3_666 3_666
Te2 Cu1 Cu1 113.17(7) 3_666 3_666
C2 C1 Te1 114.2(7) . .
C2 C1 H1A 108.7 . .
Te1 C1 H1A 108.7 . .
C2 C1 H1B 108.7 . .
Te1 C1 H1B 108.7 . .
H1A C1 H1B 107.6 . .
C1 C2 C3 115.6(9) . .
C1 C2 H2A 108.4 . .
C3 C2 H2A 108.4 . .
C1 C2 H2B 108.4 . .
C3 C2 H2B 108.4 . .
H2A C2 H2B 107.4 . .
C4 C3 C2 111.8(10) . .
C4 C3 H3A 109.3 . .
C2 C3 H3A 109.3 . .
C4 C3 H3B 109.3 . .
C2 C3 H3B 109.3 . .
H3A C3 H3B 107.9 . .
C3 C4 Te2 114.8(7) . .
C3 C4 H4A 108.6 . .
Te2 C4 H4A 108.6 . .
C3 C4 H4B 108.6 . .
Te2 C4 H4B 108.6 . .
H4A C4 H4B 107.6 . .
C11 C10 C19 119.7(10) . .
C11 C10 Te1 118.6(8) . .
C19 C10 Te1 121.4(8) . .
C10 C11 C12 122.3(10) . .
C10 C11 H11 118.8 . .
C12 C11 H11 118.8 . .
C13 C12 C11 119.8(10) . .
C13 C12 H12 120.1 . .
C11 C12 H12 120.1 . .
C12 C13 C14 120.0(11) . .
C12 C13 H13 120.0 . .
C14 C13 H13 120.0 . .
C19 C14 C15 119.0(10) . .
C19 C14 C13 119.6(9) . .
C15 C14 C13 121.4(10) . .
C16 C15 C14 120.5(11) . .
C16 C15 H15 119.7 . .
C14 C15 H15 119.7 . .
C15 C16 C17 120.2(11) . .
C15 C16 H16 119.9 . .
C17 C16 H16 119.9 . .
C18 C17 C16 121.4(11) . .
C18 C17 H17 119.3 . .
C16 C17 H17 119.3 . .
C17 C18 C19 120.1(11) . .
C17 C18 H18 120.0 . .
C19 C18 H18 120.0 . .
C14 C19 C18 118.8(9) . .
C14 C19 C10 118.5(9) . .
C18 C19 C10 122.7(10) . .
C21 C20 C29 119.1(12) . .
C21 C20 Te2 117.8(9) . .
C29 C20 Te2 122.4(9) . .
C20 C21 C22 121.0(14) . .
C20 C21 H21 119.5 . .
C22 C21 H21 119.5 . .
C23 C22 C21 120.0(14) . .
C23 C22 H22 120.0 . .
C21 C22 H22 120.0 . .
C22 C23 C24 121.3(14) . .
C22 C23 H23 119.3 . .
C24 C23 H23 119.3 . .
C23 C24 C29 118.4(14) . .
C23 C24 C25 124.0(16) . .
C29 C24 C25 117.6(15) . .
C26 C25 C24 121.0(16) . .
C26 C25 H25 119.5 . .
C24 C25 H25 119.5 . .
C25 C26 C27 121.1(16) . .
C25 C26 H26 119.4 . .
C27 C26 H26 119.4 . .
C26 C27 C28 121.3(17) . .
C26 C27 H27 119.3 . .
C28 C27 H27 119.3 . .
C27 C28 C29 121.6(14) . .
C27 C28 H28 119.2 . .
C29 C28 H28 119.2 . .
C24 C29 C20 120.0(13) . .
C24 C29 C28 117.3(12) . .
C20 C29 C28 122.7(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Te1 C10 2.132(10) .
Te1 C1 2.188(10) .
Te1 Cu1 2.5493(15) .
Te2 C20 2.105(12) .
Te2 C4 2.144(11) .
Te2 Cu1 2.5653(16) 3_666
Br1 Cu1 2.4433(18) .
Br1 Cu1 2.5495(18) 3_666
Cu1 Br1 2.5496(18) 3_666
Cu1 Te2 2.5652(16) 3_666
Cu1 Cu1 2.919(3) 3_666
C1 C2 1.509(16) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 C3 1.539(15) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.515(17) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C10 C11 1.341(15) .
C10 C19 1.431(14) .
C11 C12 1.419(16) .
C11 H11 0.9500 .
C12 C13 1.354(16) .
C12 H12 0.9500 .
C13 C14 1.429(15) .
C13 H13 0.9500 .
C14 C19 1.421(15) .
C14 C15 1.422(15) .
C15 C16 1.377(17) .
C15 H15 0.9500 .
C16 C17 1.395(16) .
C16 H16 0.9500 .
C17 C18 1.367(15) .
C17 H17 0.9500 .
C18 C19 1.429(15) .
C18 H18 0.9500 .
C20 C21 1.362(16) .
C20 C29 1.422(17) .
C21 C22 1.40(2) .
C21 H21 0.9500 .
C22 C23 1.38(2) .
C22 H22 0.9500 .
C23 C24 1.38(2) .
C23 H23 0.9500 .
C24 C29 1.422(18) .
C24 C25 1.48(2) .
C25 C26 1.35(3) .
C25 H25 0.9500 .
C26 C27 1.36(2) .
C26 H26 0.9500 .
C27 C28 1.367(18) .
C27 H27 0.9500 .
C28 C29 1.454(19) .
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 -67.8(11)
C1 C2 C3 C4 -54.7(13)
C2 C3 C4 Te2 175.9(7)
C19 C10 C11 C12 -1.7(17)
Te1 C10 C11 C12 172.0(8)
C10 C11 C12 C13 0.9(17)
C11 C12 C13 C14 -0.2(17)
C12 C13 C14 C19 0.4(16)
C12 C13 C14 C15 -178.9(10)
C19 C14 C15 C16 2.0(15)
C13 C14 C15 C16 -178.7(10)
C14 C15 C16 C17 -0.8(16)
C15 C16 C17 C18 -0.3(17)
C16 C17 C18 C19 0.2(16)
C15 C14 C19 C18 -2.1(14)
C13 C14 C19 C18 178.7(9)
C15 C14 C19 C10 178.1(9)
C13 C14 C19 C10 -1.2(14)
C17 C18 C19 C14 1.0(15)
C17 C18 C19 C10 -179.2(10)
C11 C10 C19 C14 1.9(15)
Te1 C10 C19 C14 -171.7(7)
C11 C10 C19 C18 -178.0(10)
Te1 C10 C19 C18 8.5(13)
C29 C20 C21 C22 2.3(17)
Te2 C20 C21 C22 -168.7(10)
C20 C21 C22 C23 -1(2)
C21 C22 C23 C24 -1(2)
C22 C23 C24 C29 2(2)
C22 C23 C24 C25 -179.4(13)
C23 C24 C25 C26 -177.2(14)
C29 C24 C25 C26 1.5(19)
C24 C25 C26 C27 -2(2)
C25 C26 C27 C28 1(2)
C26 C27 C28 C29 0.3(19)
C23 C24 C29 C20 -0.3(17)
C25 C24 C29 C20 -179.1(10)
C23 C24 C29 C28 178.2(11)
C25 C24 C29 C28 -0.6(16)
C21 C20 C29 C24 -1.8(16)
Te2 C20 C29 C24 168.8(8)
C21 C20 C29 C28 179.8(10)
Te2 C20 C29 C28 -9.6(15)
C27 C28 C29 C24 -0.3(17)
C27 C28 C29 C20 178.2(11)
