#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/40/7004033.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_7004033
loop_
_publ_author_name
'Martínez-Lillo, José'
'Armentano, Donatella'
'Marino, Nadia'
'Arizaga, Livia'
'Chiozzone, Raúl'
'González, Ricardo'
'Kremer, Carlos'
'Cano, Joan'
'Faus, Juan'
_publ_section_title
;
 Pentachloro(pyrazine)rhenate(iv) complex as precursor of
 heterobimetallic pyrazine-containing ReIV2MII (M = Ni, Cu) species:
 synthesis, crystal structures and magnetic properties
;
_journal_issue                   34
_journal_name_full               'Dalton Transactions'
_journal_page_first              4585
_journal_paper_doi               10.1039/b802112k
_journal_year                    2008
_chemical_formula_sum            'C10 H18 Cl5 Cu0.5 N4 O2 Re'
_chemical_formula_weight         621.50
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.3610(10)
_cell_angle_beta                 99.9690(10)
_cell_angle_gamma                102.0960(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4579(3)
_cell_length_b                   10.2914(3)
_cell_length_c                   11.8237(4)
_cell_measurement_reflns_used    5286
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      33.132
_cell_measurement_theta_min      2.283
_cell_volume                     1024.31(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'X8APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0141
_diffrn_reflns_av_sigmaI/netI    0.0166
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15185
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    7.097
_exptl_absorpt_correction_T_max  0.314
_exptl_absorpt_correction_T_min  0.276
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.015
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             593
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.750
_refine_diff_density_min         -1.053
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         6234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0187
_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)+(0.0228P)²+0.3434P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0449
_refine_ls_wR_factor_ref         0.0458
_reflns_number_gt                5840
_reflns_number_total             6234
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b802112k.txt
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C10 H18 Cl5 Cu0.50 N4 O2 Re'
_cod_database_code               7004033
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re -0.163602(8) -0.142491(8) 0.184634(7) 0.03549(3) Uani 1 1 d . . .
Cl1 Cl -0.37569(8) -0.33645(8) 0.09728(9) 0.0709(2) Uani 1 1 d . . .
Cl2 Cl -0.26432(7) -0.02576(8) 0.34483(6) 0.05471(15) Uani 1 1 d . . .
Cl3 Cl -0.05199(7) -0.24926(6) 0.30996(6) 0.04671(12) Uani 1 1 d . . .
Cl4 Cl -0.04387(7) -0.24357(7) 0.03418(5) 0.05003(13) Uani 1 1 d . . .
Cl5 Cl -0.25802(8) -0.02402(8) 0.06528(6) 0.05753(15) Uani 1 1 d . . .
N1 N 0.03742(19) 0.04152(18) 0.26964(15) 0.0322(3) Uani 1 1 d . . .
N2 N 0.2967(2) 0.2728(2) 0.38179(18) 0.0431(4) Uani 1 1 d . . .
C1 C 0.0930(2) 0.1023(2) 0.39329(19) 0.0397(4) Uani 1 1 d . . .
H1A H 0.0440 0.0670 0.4434 0.048 Uiso 1 1 calc R . .
C2 C 0.2219(3) 0.2167(2) 0.4477(2) 0.0425(5) Uani 1 1 d . . .
H2A H 0.2575 0.2558 0.5339 0.051 Uiso 1 1 calc R . .
C3 C 0.1113(3) 0.0978(2) 0.2024(2) 0.0422(5) Uani 1 1 d . . .
H3A H 0.0761 0.0591 0.1162 0.051 Uiso 1 1 calc R . .
C4 C 0.2393(3) 0.2126(3) 0.2590(2) 0.0482(6) Uani 1 1 d . . .
H4A H 0.2876 0.2495 0.2093 0.058 Uiso 1 1 calc R . .
Cu1 Cu 0.5000 0.5000 0.5000 0.03791(8) Uani 1 2 d S . .
O1 O 0.4200(2) 0.56396(18) 0.37018(15) 0.0456(4) Uani 1 1 d . . .
C5 C 0.4059(3) 0.6850(3) 0.3841(2) 0.0465(5) Uani 1 1 d . . .
H5A H 0.4484 0.7583 0.4621 0.056 Uiso 1 1 calc R . .
C6 C 0.3348(4) 0.8618(4) 0.3142(4) 0.0859(12) Uani 1 1 d . . .
H6A H 0.3879 0.9246 0.3982 0.129 Uiso 1 1 calc R . .
H6B H 0.2333 0.8664 0.2984 0.129 Uiso 1 1 calc R . .
H6C H 0.3828 0.8914 0.2580 0.129 Uiso 1 1 calc R . .
C7 C 0.2608(4) 0.6024(4) 0.1745(3) 0.0812(11) Uani 1 1 d . . .
H7A H 0.2709 0.5120 0.1758 0.122 Uiso 1 1 calc R . .
H7B H 0.3057 0.6236 0.1134 0.122 Uiso 1 1 calc R . .
H7C H 0.1564 0.5971 0.1539 0.122 Uiso 1 1 calc R . .
N3 N 0.3354(2) 0.7155(2) 0.2963(2) 0.0470(4) Uani 1 1 d . . .
O2 O 0.6428(2) 0.4301(2) 0.40969(16) 0.0491(4) Uani 1 1 d . . .
C8 C 0.6449(3) 0.4122(3) 0.3008(2) 0.0455(5) Uani 1 1 d . . .
H8A H 0.5656 0.4250 0.2511 0.055 Uiso 1 1 calc R . .
C9 C 0.7486(4) 0.3575(4) 0.1233(3) 0.0713(9) Uani 1 1 d . . .
H9A H 0.6592 0.3736 0.0851 0.107 Uiso 1 1 calc R . .
H9B H 0.7501 0.2614 0.0782 0.107 Uiso 1 1 calc R . .
H9C H 0.8348 0.4250 0.1221 0.107 Uiso 1 1 calc R . .
C10 C 0.8784(4) 0.3587(5) 0.3257(3) 0.0842(11) Uani 1 1 d . . .
H10A H 0.8670 0.3747 0.4079 0.126 Uiso 1 1 calc R . .
H10B H 0.9681 0.4266 0.3302 0.126 Uiso 1 1 calc R . .
H10C H 0.8851 0.2628 0.2877 0.126 Uiso 1 1 calc R . .
N4 N 0.7509(2) 0.3766(2) 0.2523(2) 0.0486(5) 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
Re Re -1.0185 7.2310 '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
N1 Re1 Cl1 179.33(5) . . ?
N1 Re1 Cl5 88.19(5) . . ?
Cl1 Re1 Cl5 92.26(3) . . ?
N1 Re1 Cl4 87.63(5) . . ?
Cl1 Re1 Cl4 92.87(3) . . ?
Cl5 Re1 Cl4 90.20(2) . . ?
N1 Re1 Cl2 87.55(5) . . ?
Cl1 Re1 Cl2 91.95(3) . . ?
Cl5 Re1 Cl2 90.34(3) . . ?
Cl4 Re1 Cl2 175.12(2) . . ?
N1 Re1 Cl3 87.79(5) . . ?
Cl1 Re1 Cl3 91.77(3) . . ?
Cl5 Re1 Cl3 175.94(2) . . ?
Cl4 Re1 Cl3 89.06(2) . . ?
Cl2 Re1 Cl3 90.06(2) . . ?
C3 N1 C1 116.87(18) . . ?
C3 N1 Re1 122.40(14) . . ?
C1 N1 Re1 120.73(13) . . ?
C2 N2 C4 115.84(19) . . ?
C2 N2 Cu1 116.50(14) . . ?
C4 N2 Cu1 126.82(15) . . ?
N1 C1 C2 121.13(19) . . ?
N1 C1 H1A 119.4 . . ?
C2 C1 H1A 119.4 . . ?
N2 C2 C1 122.5(2) . . ?
N2 C2 H2A 118.8 . . ?
C1 C2 H2A 118.8 . . ?
N1 C3 C4 120.9(2) . . ?
N1 C3 H3A 119.6 . . ?
C4 C3 H3A 119.6 . . ?
N2 C4 C3 122.8(2) . . ?
N2 C4 H4A 118.6 . . ?
C3 C4 H4A 118.6 . . ?
O1 Cu1 O1 180.0 2_666 . ?
O1 Cu1 O2 88.95(7) 2_666 . ?
O1 Cu1 O2 91.05(7) . . ?
O1 Cu1 O2 91.05(7) 2_666 2_666 ?
O1 Cu1 O2 88.95(7) . 2_666 ?
O2 Cu1 O2 180.0 . 2_666 ?
O1 Cu1 N2 94.46(7) 2_666 . ?
O1 Cu1 N2 85.54(7) . . ?
O2 Cu1 N2 92.82(7) . . ?
O2 Cu1 N2 87.18(7) 2_666 . ?
O1 Cu1 N2 85.54(7) 2_666 2_666 ?
O1 Cu1 N2 94.46(7) . 2_666 ?
O2 Cu1 N2 87.18(7) . 2_666 ?
O2 Cu1 N2 92.82(7) 2_666 2_666 ?
N2 Cu1 N2 180.00(8) . 2_666 ?
C5 O1 Cu1 127.19(16) . . ?
O1 C5 N3 123.9(2) . . ?
O1 C5 H5A 118.0 . . ?
N3 C5 H5A 118.0 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N3 C7 H7A 109.5 . . ?
N3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 N3 C6 121.6(3) . . ?
C5 N3 C7 119.9(2) . . ?
C6 N3 C7 118.5(3) . . ?
C8 O2 Cu1 128.45(17) . . ?
O2 C8 N4 123.9(2) . . ?
O2 C8 H8A 118.0 . . ?
N4 C8 H8A 118.0 . . ?
N4 C9 H9A 109.5 . . ?
N4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N4 C10 H10A 109.5 . . ?
N4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 N4 C10 120.6(2) . . ?
C8 N4 C9 121.8(2) . . ?
C10 N4 C9 117.6(2) . . ?
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
Re1 N1 2.1860(16) . ?
Re1 Cl1 2.3049(6) . ?
Re1 Cl5 2.3315(6) . ?
Re1 Cl4 2.3437(6) . ?
Re1 Cl2 2.3524(6) . ?
Re1 Cl3 2.3541(6) . ?
N1 C3 1.336(3) . ?
N1 C1 1.340(3) . ?
N2 C2 1.327(3) . ?
N2 C4 1.333(3) . ?
N2 Cu1 2.4769(18) . ?
C1 C2 1.383(3) . ?
C1 H1A 0.9300 . ?
C2 H2A 0.9300 . ?
C3 C4 1.380(3) . ?
C3 H3A 0.9300 . ?
C4 H4A 0.9300 . ?
Cu1 O1 1.9593(15) 2_666 ?
Cu1 O1 1.9593(15) . ?
Cu1 O2 1.9691(17) . ?
Cu1 O2 1.9691(17) 2_666 ?
Cu1 N2 2.4769(18) 2_666 ?
O1 C5 1.240(3) . ?
C5 N3 1.298(3) . ?
C5 H5A 0.9300 . ?
C6 N3 1.451(4) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 N3 1.456(4) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
O2 C8 1.243(3) . ?
C8 N4 1.297(3) . ?
C8 H8A 0.9300 . ?
C9 N4 1.468(3) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 N4 1.441(4) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
