#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:34:10 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179754 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/50/7005084.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_7005084
loop_
_publ_author_name
'Kennedy, Frazer'
'Shavaleev, Nail M.'
'Koullourou, Thelma'
'Bell, Zoë R'
'Jeffery, John C.'
'Faulkner, Stephen'
'Ward, Michael D.'
_publ_section_title
;
 Sensitised near-infrared luminescence from lanthanide(III) centres
 using Re(I) and Pt(II) diimine complexes as energy donors in d-f
 dinuclear complexes based on 2,3-bis(2-pyridyl)pyrazine.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1492
_journal_page_last               1499
_journal_paper_doi               10.1039/b616423d
_journal_year                    2007
_chemical_formula_sum            'C18 H11 Cl4 N4 O3 Re'
_chemical_formula_weight         659.31
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.969(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.4657(16)
_cell_length_b                   19.437(5)
_cell_length_c                   17.053(4)
_cell_measurement_temperature    173(2)
_cell_volume                     2135.1(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Siemens SMART area detector'
_diffrn_measurement_method       'ω rotation with narrow frames'
_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  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11953
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    6.220
_exptl_absorpt_correction_T_max  0.49
_exptl_absorpt_correction_T_min  0.14
_exptl_absorpt_correction_type   'Empirical, pseudo-azimuthal scan (SADABS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.051
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.378
_refine_diff_density_min         -0.919
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0446P)²+2.4169P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                3670
_reflns_number_total             4571
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b616423d.txt
_cod_data_source_block           larges
_cod_original_cell_volume        2135.0(9)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7005084
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.41627(3) 0.726113(11) 0.199337(12) 0.02027(9) Uani 1 1 d . . .
Cl1 Cl 0.6053(2) 0.83324(8) 0.23360(9) 0.0330(3) Uani 1 1 d . . .
Cl11 Cl 0.5875(6) 0.50439(14) 0.14898(16) 0.1105(13) Uani 1 1 d . . .
Cl12 Cl 0.9429(4) 0.41490(14) 0.17491(16) 0.0747(7) Uani 1 1 d . . .
Cl13 Cl 0.6823(4) 0.40952(15) 0.02966(14) 0.0744(7) Uani 1 1 d . . .
O41 O 0.1667(8) 0.5976(3) 0.1547(3) 0.0494(13) Uani 1 1 d . . .
O51 O 0.1553(8) 0.7388(2) 0.3411(3) 0.0395(12) Uani 1 1 d . . .
O61 O 0.7516(7) 0.6443(2) 0.2975(3) 0.0364(10) Uani 1 1 d . . .
N11 N 0.5771(7) 0.7264(2) 0.0927(3) 0.0235(10) Uani 1 1 d . . .
N21 N 0.2366(7) 0.7927(2) 0.1180(2) 0.0185(9) Uani 1 1 d . . .
N24 N 0.0523(7) 0.8925(2) 0.0202(3) 0.0252(10) Uani 1 1 d . . .
N31 N 0.5484(7) 0.9213(2) -0.0306(3) 0.0223(10) Uani 1 1 d . . .
C12 C 0.5057(8) 0.7696(3) 0.0345(3) 0.0187(11) Uani 1 1 d . . .
C13 C 0.5863(9) 0.7682(3) -0.0390(4) 0.0249(12) Uani 1 1 d . . .
H13A H 0.5309 0.7973 -0.0804 0.030 Uiso 1 1 calc R . .
C14 C 0.7492(10) 0.7236(3) -0.0502(4) 0.0308(14) Uani 1 1 d . . .
H14A H 0.8073 0.7223 -0.0995 0.037 Uiso 1 1 calc R . .
C15 C 0.8264(9) 0.6811(3) 0.0103(4) 0.0321(14) Uani 1 1 d . . .
H15A H 0.9393 0.6510 0.0038 0.038 Uiso 1 1 calc R . .
C16 C 0.7359(9) 0.6835(3) 0.0802(4) 0.0291(13) Uani 1 1 d . . .
H16A H 0.7870 0.6538 0.1216 0.035 Uiso 1 1 calc R . .
C22 C 0.3252(8) 0.8126(3) 0.0514(3) 0.0189(10) Uani 1 1 d . . .
C23 C 0.2404(8) 0.8679(3) 0.0073(3) 0.0211(11) Uani 1 1 d . . .
C25 C -0.0431(9) 0.8681(3) 0.0804(3) 0.0266(12) Uani 1 1 d . . .
H25A H -0.1799 0.8831 0.0878 0.032 Uiso 1 1 calc R . .
C26 C 0.0543(8) 0.8209(3) 0.1330(3) 0.0228(11) Uani 1 1 d . . .
H26A H -0.0082 0.8086 0.1794 0.027 Uiso 1 1 calc R . .
C32 C 0.3491(9) 0.9080(3) -0.0514(3) 0.0226(11) Uani 1 1 d . . .
C33 C 0.2375(9) 0.9355(3) -0.1179(3) 0.0275(12) Uani 1 1 d . . .
H33A H 0.0962 0.9236 -0.1308 0.033 Uiso 1 1 calc R . .
C34 C 0.3384(10) 0.9806(3) -0.1645(4) 0.0310(14) Uani 1 1 d . . .
H34A H 0.2685 1.0004 -0.2104 0.037 Uiso 1 1 calc R . .
C35 C 0.5439(10) 0.9959(3) -0.1423(3) 0.0300(13) Uani 1 1 d . . .
H35A H 0.6165 1.0278 -0.1720 0.036 Uiso 1 1 calc R . .
C36 C 0.6434(9) 0.9646(3) -0.0767(3) 0.0262(12) Uani 1 1 d . . .
H36A H 0.7863 0.9743 -0.0637 0.031 Uiso 1 1 calc R . .
C41 C 0.2542(8) 0.6417(3) 0.1651(4) 0.0211(12) Uani 1 1 d . . .
C51 C 0.2502(10) 0.7338(3) 0.2870(4) 0.0267(13) Uani 1 1 d . . .
C61 C 0.6220(9) 0.6730(3) 0.2621(3) 0.0282(13) Uani 1 1 d . . .
C100 C 0.6882(13) 0.4247(4) 0.1304(5) 0.052(2) Uani 1 1 d . . .
H100 H 0.5989 0.3893 0.1534 0.063 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'
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'
F F 0.0171 0.0103 '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'
Nd Nd -0.1943 3.0179 '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
C51 Re1 C61 90.8(2) . . ?
C51 Re1 C41 88.7(2) . . ?
C61 Re1 C41 92.4(2) . . ?
C51 Re1 N21 98.5(2) . . ?
C61 Re1 N21 169.0(2) . . ?
C41 Re1 N21 93.72(19) . . ?
C51 Re1 N11 172.9(2) . . ?
C61 Re1 N11 96.2(2) . . ?
C41 Re1 N11 92.0(2) . . ?
N21 Re1 N11 74.38(17) . . ?
C51 Re1 Cl1 92.83(19) . . ?
C61 Re1 Cl1 90.93(18) . . ?
C41 Re1 Cl1 176.33(15) . . ?
N21 Re1 Cl1 82.75(13) . . ?
N11 Re1 Cl1 86.11(13) . . ?
C12 N11 C16 118.8(5) . . ?
C12 N11 Re1 117.3(4) . . ?
C16 N11 Re1 123.7(4) . . ?
C26 N21 C22 118.6(5) . . ?
C26 N21 Re1 123.6(4) . . ?
C22 N21 Re1 117.4(3) . . ?
C25 N24 C23 119.1(5) . . ?
C32 N31 C36 116.6(5) . . ?
N11 C12 C13 121.1(5) . . ?
N11 C12 C22 115.6(5) . . ?
C13 C12 C22 123.0(5) . . ?
C14 C13 C12 118.8(5) . . ?
C14 C13 H13A 120.6 . . ?
C12 C13 H13A 120.6 . . ?
C15 C14 C13 119.9(6) . . ?
C15 C14 H14A 120.1 . . ?
C13 C14 H14A 120.1 . . ?
C16 C15 C14 118.4(6) . . ?
C16 C15 H15A 120.8 . . ?
C14 C15 H15A 120.8 . . ?
N11 C16 C15 123.0(6) . . ?
N11 C16 H16A 118.5 . . ?
C15 C16 H16A 118.5 . . ?
N21 C22 C23 119.3(5) . . ?
N21 C22 C12 113.2(4) . . ?
C23 C22 C12 127.4(5) . . ?
N24 C23 C22 120.3(5) . . ?
N24 C23 C32 114.2(5) . . ?
C22 C23 C32 125.3(5) . . ?
N24 C25 C26 121.2(5) . . ?
N24 C25 H25A 119.4 . . ?
C26 C25 H25A 119.4 . . ?
N21 C26 C25 120.0(5) . . ?
N21 C26 H26A 120.0 . . ?
C25 C26 H26A 120.0 . . ?
N31 C32 C33 124.2(5) . . ?
N31 C32 C23 115.0(5) . . ?
C33 C32 C23 120.4(5) . . ?
C34 C33 C32 118.3(6) . . ?
C34 C33 H33A 120.9 . . ?
C32 C33 H33A 120.9 . . ?
C35 C34 C33 117.9(6) . . ?
C35 C34 H34A 121.0 . . ?
C33 C34 H34A 121.0 . . ?
C36 C35 C34 119.7(6) . . ?
C36 C35 H35A 120.1 . . ?
C34 C35 H35A 120.1 . . ?
N31 C36 C35 123.2(6) . . ?
N31 C36 H36A 118.4 . . ?
C35 C36 H36A 118.4 . . ?
O41 C41 Re1 172.9(6) . . ?
O51 C51 Re1 178.0(6) . . ?
O61 C61 Re1 176.0(5) . . ?
Cl11 C100 Cl13 111.0(4) . . ?
Cl11 C100 Cl12 111.8(5) . . ?
Cl13 C100 Cl12 110.3(4) . . ?
Cl11 C100 H100 107.8 . . ?
Cl13 C100 H100 107.8 . . ?
Cl12 C100 H100 107.8 . . ?
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 C51 1.920(6) . ?
Re1 C61 1.932(6) . ?
Re1 C41 2.006(6) . ?
Re1 N21 2.161(4) . ?
Re1 N11 2.171(5) . ?
Re1 Cl1 2.4592(16) . ?
Cl11 C100 1.721(8) . ?
Cl12 C100 1.763(9) . ?
Cl13 C100 1.740(8) . ?
O41 C41 1.034(7) . ?
O51 C51 1.156(8) . ?
O61 C61 1.136(7) . ?
N11 C12 1.350(7) . ?
N11 C16 1.354(7) . ?
N21 C26 1.344(7) . ?
N21 C22 1.371(7) . ?
N24 C25 1.330(7) . ?
N24 C23 1.343(7) . ?
N31 C32 1.332(7) . ?
N31 C36 1.337(7) . ?
C12 C13 1.399(8) . ?
C12 C22 1.483(7) . ?
C13 C14 1.391(8) . ?
C13 H13A 0.9500 . ?
C14 C15 1.381(9) . ?
C14 H14A 0.9500 . ?
C15 C16 1.373(8) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
C22 C23 1.396(7) . ?
C23 C32 1.492(7) . ?
C25 C26 1.394(8) . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9500 . ?
C32 C33 1.397(8) . ?
C33 C34 1.383(8) . ?
C33 H33A 0.9500 . ?
C34 C35 1.383(9) . ?
C34 H34A 0.9500 . ?
C35 C36 1.383(8) . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?
C100 H100 1.0000 . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C51 Re1 N11 C12 4(2) . . . . ?
C61 Re1 N11 C12 -168.2(4) . . . . ?
C41 Re1 N11 C12 99.2(4) . . . . ?
N21 Re1 N11 C12 5.9(4) . . . . ?
Cl1 Re1 N11 C12 -77.7(4) . . . . ?
C51 Re1 N11 C16 -172.3(17) . . . . ?
C61 Re1 N11 C16 15.5(5) . . . . ?
C41 Re1 N11 C16 -77.2(5) . . . . ?
N21 Re1 N11 C16 -170.5(5) . . . . ?
Cl1 Re1 N11 C16 106.0(5) . . . . ?
C51 Re1 N21 C26 -5.6(5) . . . . ?
C61 Re1 N21 C26 -152.9(10) . . . . ?
C41 Re1 N21 C26 83.6(4) . . . . ?
N11 Re1 N21 C26 174.7(5) . . . . ?
Cl1 Re1 N21 C26 -97.4(4) . . . . ?
C51 Re1 N21 C22 167.5(4) . . . . ?
C61 Re1 N21 C22 20.2(13) . . . . ?
C41 Re1 N21 C22 -103.3(4) . . . . ?
N11 Re1 N21 C22 -12.3(4) . . . . ?
Cl1 Re1 N21 C22 75.7(4) . . . . ?
C16 N11 C12 C13 3.0(8) . . . . ?
Re1 N11 C12 C13 -173.5(4) . . . . ?
C16 N11 C12 C22 177.2(5) . . . . ?
Re1 N11 C12 C22 0.7(6) . . . . ?
N11 C12 C13 C14 -3.0(9) . . . . ?
C22 C12 C13 C14 -176.7(5) . . . . ?
C12 C13 C14 C15 0.8(9) . . . . ?
C13 C14 C15 C16 1.2(10) . . . . ?
C12 N11 C16 C15 -1.0(9) . . . . ?
Re1 N11 C16 C15 175.3(5) . . . . ?
C14 C15 C16 N11 -1.2(10) . . . . ?
C26 N21 C22 C23 9.0(8) . . . . ?
Re1 N21 C22 C23 -164.4(4) . . . . ?
C26 N21 C22 C12 -170.2(5) . . . . ?
Re1 N21 C22 C12 16.4(6) . . . . ?
N11 C12 C22 N21 -11.0(7) . . . . ?
C13 C12 C22 N21 163.0(5) . . . . ?
N11 C12 C22 C23 169.8(5) . . . . ?
C13 C12 C22 C23 -16.1(9) . . . . ?
C25 N24 C23 C22 6.5(8) . . . . ?
C25 N24 C23 C32 -168.8(5) . . . . ?
N21 C22 C23 N24 -13.3(8) . . . . ?
C12 C22 C23 N24 165.8(5) . . . . ?
N21 C22 C23 C32 161.5(5) . . . . ?
C12 C22 C23 C32 -19.4(9) . . . . ?
C23 N24 C25 C26 4.1(8) . . . . ?
C22 N21 C26 C25 1.4(8) . . . . ?
Re1 N21 C26 C25 174.3(4) . . . . ?
N24 C25 C26 N21 -8.3(9) . . . . ?
C36 N31 C32 C33 0.9(8) . . . . ?
C36 N31 C32 C23 -171.5(5) . . . . ?
N24 C23 C32 N31 134.8(5) . . . . ?
C22 C23 C32 N31 -40.2(8) . . . . ?
N24 C23 C32 C33 -37.8(7) . . . . ?
C22 C23 C32 C33 147.1(6) . . . . ?
N31 C32 C33 C34 -1.3(9) . . . . ?
C23 C32 C33 C34 170.6(5) . . . . ?
C32 C33 C34 C35 -0.2(9) . . . . ?
C33 C34 C35 C36 2.1(9) . . . . ?
C32 N31 C36 C35 1.1(8) . . . . ?
C34 C35 C36 N31 -2.6(9) . . . . ?
C51 Re1 C41 O41 -24(4) . . . . ?
C61 Re1 C41 O41 67(4) . . . . ?
N21 Re1 C41 O41 -122(4) . . . . ?
N11 Re1 C41 O41 163(4) . . . . ?
Cl1 Re1 C41 O41 -138(3) . . . . ?
C61 Re1 C51 O51 44(15) . . . . ?
C41 Re1 C51 O51 136(15) . . . . ?
N21 Re1 C51 O51 -130(15) . . . . ?
N11 Re1 C51 O51 -128(15) . . . . ?
Cl1 Re1 C51 O51 -47(15) . . . . ?
C51 Re1 C61 O61 -132(8) . . . . ?
C41 Re1 C61 O61 139(8) . . . . ?
N21 Re1 C61 O61 16(9) . . . . ?
N11 Re1 C61 O61 47(8) . . . . ?
Cl1 Re1 C61 O61 -39(8) . . . . ?
