#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:52:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179159 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/20/4312051.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_4312051
loop_
_publ_author_name
'Michael Q. Dequeant'
'Patricia M. Bradley'
'Guo-Lin Xu'
'Daniel A. Lutterman'
'Claudia Turro'
'Tong Ren'
_publ_contact_author_address
; Department of Chemistry 
  University of Miami 
  PO BOX 249118 
  Coral Gables, FL 33124-0431 
  USA 
;
_publ_contact_author_email       tren@miami.edu
_publ_contact_author_fax         '(305) 284-1880'
_publ_contact_author_name        'Dr. Ren, Tong'
_publ_contact_author_phone       '(305) 284-6617'
_publ_section_title
;
 Dirhenium Paddlewheel Compounds Supported by N,N'-Dialkylbenzamidinates:
 Synthesis, Structures, and Photophysical Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7887
_journal_page_last               7892
_journal_paper_doi               10.1021/ic0487981
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C36 H44 Cl2 N8 Re2'
_chemical_formula_weight         1032.09
_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                104.589(2)
_cell_angle_beta                 113.628(2)
_cell_angle_gamma                102.727(2)
_cell_formula_units_Z            1
_cell_length_a                   9.5810(9)
_cell_length_b                   10.2213(9)
_cell_length_c                   11.6178(11)
_cell_measurement_reflns_used    3565
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      27.770
_cell_measurement_theta_min      2.209
_cell_volume                     940.20(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      300(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  '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  0.1260
_diffrn_reflns_av_sigmaI/netI    0.1185
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4901
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    6.611
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.247695
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
  SADABS, Absorption corrections using Bruker CCD based on the method of 
  Bob Blessing.  Acta Cryst. 1995, A51, 33 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.830
_refine_diff_density_min         -4.083
_refine_diff_density_rms         0.304
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         3263
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0639
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0900P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1619
_reflns_number_gt                2604
_reflns_number_total             3263
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0487981si20040830_100947_1.cif
_cod_data_source_block           compd01
_cod_database_code               4312051
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 0.97213(6) 0.59679(5) 0.53612(5) 0.0349(2) Uani 1 1 d . . .
Cl1 Cl 0.8995(5) 0.8228(3) 0.6243(4) 0.0536(9) Uani 1 1 d . . .
N2 N 1.0586(14) 0.6977(10) 0.4307(10) 0.040(2) Uani 1 1 d . . .
N4 N 0.8816(13) 0.5027(11) 0.6456(10) 0.039(2) Uani 1 1 d . . .
N1 N 1.2026(13) 0.6948(10) 0.7036(11) 0.037(2) Uani 1 1 d . . .
N3 N 0.7406(13) 0.5064(11) 0.3675(12) 0.043(3) Uani 1 1 d . . .
C1 C 1.261(2) 0.8465(13) 0.8032(14) 0.054(4) Uani 1 1 d . . .
H1A H 1.3708 0.8720 0.8733 0.081 Uiso 1 1 calc R . .
H1B H 1.1910 0.8521 0.8430 0.081 Uiso 1 1 calc R . .
H1C H 1.2592 0.9125 0.7572 0.081 Uiso 1 1 calc R . .
C2 C 1.067(2) 0.8454(15) 0.4387(16) 0.058(4) Uani 1 1 d . . .
H2A H 1.1103 0.8709 0.3825 0.087 Uiso 1 1 calc R . .
H2B H 1.1368 0.9125 0.5311 0.087 Uiso 1 1 calc R . .
H2C H 0.9594 0.8492 0.4077 0.087 Uiso 1 1 calc R . .
C3 C 0.624(2) 0.5829(17) 0.3430(19) 0.075(5) Uani 1 1 d . . .
H3A H 0.5248 0.5226 0.2600 0.112 Uiso 1 1 calc R . .
H3B H 0.6711 0.6718 0.3359 0.112 Uiso 1 1 calc R . .
H3C H 0.6006 0.6041 0.4171 0.112 Uiso 1 1 calc R . .
C4 C 0.811(2) 0.5747(16) 0.7212(17) 0.063(4) Uani 1 1 d . . .
H4A H 0.7766 0.5153 0.7642 0.094 Uiso 1 1 calc R . .
H4B H 0.7181 0.5892 0.6599 0.094 Uiso 1 1 calc R . .
H4C H 0.8911 0.6668 0.7892 0.094 Uiso 1 1 calc R . .
C5 C 0.6905(16) 0.3731(12) 0.2775(12) 0.036(3) Uiso 1 1 d . . .
C6 C 0.8774(16) 0.3707(12) 0.6371(12) 0.036(3) Uiso 1 1 d . . .
C7 C 0.5210(17) 0.3004(13) 0.1645(13) 0.044(3) Uani 1 1 d . . .
C8 C 0.478(2) 0.3137(19) 0.0401(16) 0.066(4) Uani 1 1 d . . .
H8A H 0.5569 0.3715 0.0280 0.079 Uiso 1 1 calc R . .
C9 C 0.322(3) 0.242(2) -0.0653(19) 0.097(7) Uani 1 1 d . . .
H9A H 0.2943 0.2517 -0.1485 0.117 Uiso 1 1 calc R . .
C10 C 0.202(2) 0.1558(18) -0.048(2) 0.073(5) Uani 1 1 d . . .
H10A H 0.0967 0.1051 -0.1200 0.087 Uiso 1 1 calc R . .
C11 C 0.242(2) 0.1464(17) 0.0750(18) 0.069(5) Uani 1 1 d . . .
H11A H 0.1637 0.0909 0.0884 0.083 Uiso 1 1 calc R . .
C12 C 0.399(2) 0.2191(15) 0.1789(16) 0.059(4) Uani 1 1 d . . .
H12A H 0.4240 0.2133 0.2631 0.071 Uiso 1 1 calc R . .
C13 C 0.7953(16) 0.2966(13) 0.7008(14) 0.042(3) Uani 1 1 d . . .
C14 C 0.629(2) 0.2132(16) 0.6296(17) 0.062(4) Uani 1 1 d . . .
H14A H 0.5684 0.2050 0.5408 0.074 Uiso 1 1 calc R . .
C15 C 0.551(2) 0.1419(17) 0.687(2) 0.077(5) Uani 1 1 d . . .
H15A H 0.4400 0.0867 0.6371 0.092 Uiso 1 1 calc R . .
C16 C 0.642(3) 0.155(2) 0.817(2) 0.087(7) Uani 1 1 d . . .
H16A H 0.5922 0.1041 0.8557 0.104 Uiso 1 1 calc R . .
C17 C 0.802(3) 0.239(2) 0.891(2) 0.098(7) Uani 1 1 d . . .
H17A H 0.8590 0.2507 0.9818 0.117 Uiso 1 1 calc R . .
C18 C 0.883(2) 0.3106(18) 0.8349(17) 0.074(5) Uani 1 1 d . . .
H18A H 0.9940 0.3663 0.8863 0.088 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'
Cl Cl 0.1484 0.1585 '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 N3 177.7(4) . . ?
N1 Re1 N2 89.5(4) . . ?
N3 Re1 N2 89.1(4) . . ?
N1 Re1 N4 90.6(4) . . ?
N3 Re1 N4 90.7(4) . . ?
N2 Re1 N4 177.4(4) . . ?
N1 Re1 Re1 91.0(3) . 2_766 ?
N3 Re1 Re1 90.9(3) . 2_766 ?
N2 Re1 Re1 92.3(3) . 2_766 ?
N4 Re1 Re1 90.3(3) . 2_766 ?
N1 Re1 Cl1 89.5(3) . . ?
N3 Re1 Cl1 88.6(3) . . ?
N2 Re1 Cl1 89.4(3) . . ?
N4 Re1 Cl1 88.0(3) . . ?
Re1 Re1 Cl1 178.21(8) 2_766 . ?
C6 N2 C2 119.0(11) 2_766 . ?
C6 N2 Re1 117.7(8) 2_766 . ?
C2 N2 Re1 123.0(9) . . ?
C6 N4 C4 119.2(11) . . ?
C6 N4 Re1 118.8(9) . . ?
C4 N4 Re1 121.8(9) . . ?
C5 N1 C1 117.3(12) 2_766 . ?
C5 N1 Re1 120.4(8) 2_766 . ?
C1 N1 Re1 122.2(9) . . ?
C5 N3 C3 117.2(12) . . ?
C5 N3 Re1 120.1(9) . . ?
C3 N3 Re1 122.7(9) . . ?
N3 C5 N1 117.5(12) . 2_766 ?
N3 C5 C7 121.2(12) . . ?
N1 C5 C7 121.2(10) 2_766 . ?
N4 C6 N2 120.7(11) . 2_766 ?
N4 C6 C13 119.0(12) . . ?
N2 C6 C13 120.3(11) 2_766 . ?
C12 C7 C8 117.4(14) . . ?
C12 C7 C5 121.4(13) . . ?
C8 C7 C5 121.2(13) . . ?
C9 C8 C7 120.6(17) . . ?
C8 C9 C10 120.1(18) . . ?
C11 C10 C9 119.4(16) . . ?
C10 C11 C12 119.5(16) . . ?
C11 C12 C7 122.9(15) . . ?
C14 C13 C18 117.9(13) . . ?
C14 C13 C6 121.5(13) . . ?
C18 C13 C6 120.7(13) . . ?
C13 C14 C15 122.2(17) . . ?
C16 C15 C14 118.5(17) . . ?
C17 C16 C15 120.8(16) . . ?
C16 C17 C18 121(2) . . ?
C13 C18 C17 119.1(18) . . ?
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 2.065(11) . ?
Re1 N3 2.077(11) . ?
Re1 N2 2.079(10) . ?
Re1 N4 2.104(10) . ?
Re1 Re1 2.2120(9) 2_766 ?
Re1 Cl1 2.637(4) . ?
N2 C6 1.335(17) 2_766 ?
N2 C2 1.471(17) . ?
N4 C6 1.318(16) . ?
N4 C4 1.466(18) . ?
N1 C5 1.338(17) 2_766 ?
N1 C1 1.500(14) . ?
N3 C5 1.331(15) . ?
N3 C3 1.476(18) . ?
C5 N1 1.338(17) 2_766 ?
C5 C7 1.476(18) . ?
C6 N2 1.335(17) 2_766 ?
C6 C13 1.493(17) . ?
C7 C12 1.373(19) . ?
C7 C8 1.387(19) . ?
C8 C9 1.37(3) . ?
C9 C10 1.40(3) . ?
C10 C11 1.36(2) . ?
C11 C12 1.37(2) . ?
C13 C14 1.390(19) . ?
C13 C18 1.39(2) . ?
C14 C15 1.39(2) . ?
C15 C16 1.37(3) . ?
C16 C17 1.35(3) . ?
C17 C18 1.41(2) . ?
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
N1 Re1 N2 C6 88.2(9) . . . 2_766 ?
N3 Re1 N2 C6 -93.7(9) . . . 2_766 ?
N4 Re1 N2 C6 -180(100) . . . 2_766 ?
Re1 Re1 N2 C6 -2.8(9) 2_766 . . 2_766 ?
Cl1 Re1 N2 C6 177.7(9) . . . 2_766 ?
N1 Re1 N2 C2 -85.6(11) . . . . ?
N3 Re1 N2 C2 92.6(11) . . . . ?
N4 Re1 N2 C2 7(9) . . . . ?
Re1 Re1 N2 C2 -176.6(11) 2_766 . . . ?
Cl1 Re1 N2 C2 4.0(11) . . . . ?
N1 Re1 N4 C6 -93.6(10) . . . . ?
N3 Re1 N4 C6 88.3(10) . . . . ?
N2 Re1 N4 C6 174(8) . . . . ?
Re1 Re1 N4 C6 -2.5(9) 2_766 . . . ?
Cl1 Re1 N4 C6 176.9(9) . . . . ?
N1 Re1 N4 C4 91.7(11) . . . . ?
N3 Re1 N4 C4 -86.4(11) . . . . ?
N2 Re1 N4 C4 -1(9) . . . . ?
Re1 Re1 N4 C4 -177.3(11) 2_766 . . . ?
Cl1 Re1 N4 C4 2.2(11) . . . . ?
N3 Re1 N1 C5 -145(9) . . . 2_766 ?
N2 Re1 N1 C5 -92.3(9) . . . 2_766 ?
N4 Re1 N1 C5 90.3(10) . . . 2_766 ?
Re1 Re1 N1 C5 -0.1(9) 2_766 . . 2_766 ?
Cl1 Re1 N1 C5 178.2(9) . . . 2_766 ?
N3 Re1 N1 C1 31(10) . . . . ?
N2 Re1 N1 C1 83.7(10) . . . . ?
N4 Re1 N1 C1 -93.7(10) . . . . ?
Re1 Re1 N1 C1 176.0(9) 2_766 . . . ?
Cl1 Re1 N1 C1 -5.7(9) . . . . ?
N1 Re1 N3 C5 148(9) . . . . ?
N2 Re1 N3 C5 95.4(10) . . . . ?
N4 Re1 N3 C5 -87.2(10) . . . . ?
Re1 Re1 N3 C5 3.1(9) 2_766 . . . ?
Cl1 Re1 N3 C5 -175.2(9) . . . . ?
N1 Re1 N3 C3 -33(10) . . . . ?
N2 Re1 N3 C3 -86.1(12) . . . . ?
N4 Re1 N3 C3 91.3(12) . . . . ?
Re1 Re1 N3 C3 -178.3(12) 2_766 . . . ?
Cl1 Re1 N3 C3 3.4(12) . . . . ?
C3 N3 C5 N1 177.7(12) . . . 2_766 ?
Re1 N3 C5 N1 -3.7(16) . . . 2_766 ?
C3 N3 C5 C7 -5.0(19) . . . . ?
Re1 N3 C5 C7 173.7(9) . . . . ?
C4 N4 C6 N2 -179.7(11) . . . 2_766 ?
Re1 N4 C6 N2 5.4(16) . . . 2_766 ?
C4 N4 C6 C13 2(2) . . . . ?
Re1 N4 C6 C13 -172.8(9) . . . . ?
N3 C5 C7 C12 -88.6(16) . . . . ?
N1 C5 C7 C12 88.7(17) 2_766 . . . ?
N3 C5 C7 C8 90.4(17) . . . . ?
N1 C5 C7 C8 -92.4(16) 2_766 . . . ?
C12 C7 C8 C9 -3(2) . . . . ?
C5 C7 C8 C9 178.2(17) . . . . ?
C7 C8 C9 C10 0(3) . . . . ?
C8 C9 C10 C11 2(3) . . . . ?
C9 C10 C11 C12 -1(3) . . . . ?
C10 C11 C12 C7 -1(3) . . . . ?
C8 C7 C12 C11 3(2) . . . . ?
C5 C7 C12 C11 -177.6(15) . . . . ?
N4 C6 C13 C14 88.8(16) . . . . ?
N2 C6 C13 C14 -89.3(17) 2_766 . . . ?
N4 C6 C13 C18 -90.3(18) . . . . ?
N2 C6 C13 C18 91.5(17) 2_766 . . . ?
C18 C13 C14 C15 -2(2) . . . . ?
C6 C13 C14 C15 179.1(14) . . . . ?
C13 C14 C15 C16 0(3) . . . . ?
C14 C15 C16 C17 3(3) . . . . ?
C15 C16 C17 C18 -4(3) . . . . ?
C14 C13 C18 C17 1(3) . . . . ?
C6 C13 C18 C17 179.9(16) . . . . ?
C16 C17 C18 C13 2(3) . . . . ?
