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#$Date: 2016-03-23 15:06:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179313 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/10/4321002.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_4321002
loop_
_publ_author_name
'Yan Ding'
'Shan-Ming Kuang'
'Michael J. Siwajek'
'Phillip E. Fanwick'
'Richard A. Walton'
_publ_contact_author_address
;    Department of Chemistry
     Purdue University
     W. Lafayette
     IN 47907
     USA
;
_publ_contact_author_email       fanwick@.xray.chem.purdue.edu
_publ_contact_author_fax         1(765)4940239
_publ_contact_author_name        'Phillip E. Fanwick'
_publ_contact_author_phone       1(765)4944572
_publ_section_title
;
 Reactions of the Dirhenium(II) Complexes Re2X4(μ-dppm)2 (X = Cl, Br;
 dppm = Ph2PCH2PPh2) with Isocyanides. 21.1A Comparison with the Complexes
 Re2Cl4(μ-dppE)2 and Re2Cl4(μ-dcpm)2 (dppE = Ph2PC(CH2)PPh2; dcpm =
 Cy2PCH2PCy2) and the Structural Characterization of Complexes of the
 Types Re2Cl4(μ-LL)2(CNR), Re2Cl4(μ-LL)2(CNR)2, and
 [Re2Cl3(μ-LL)2(CNR)3]+ (LL = dppm, dppE, dcpm; R =t-Bu, Xyl)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2676
_journal_page_last               2683
_journal_paper_doi               10.1021/ic000064a
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         'C59 H53 Cl4 N1 P4 Re2'
_chemical_formula_sum            'C59 H53 Cl4 N P4 Re2'
_chemical_formula_weight         1414.1
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0903(4)
_cell_length_b                   15.0903(4)
_cell_length_c                   26.1521(7)
_cell_measurement_temperature    203(2)
_cell_volume                     5955.3(3)
_computing_cell_refinement       DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_data_collection       Collect_(Nonius,_1998)
_computing_data_reduction        DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_molecular_graphics    Ortep-3_for_Windows_(Farrugia,_1997)
_computing_publication_material  WinGX_publication_routines_(Farrugia,_1998)
_computing_structure_refinement  SHELXL97_(Sheldrick,_1997)
_computing_structure_solution    SHELXS97_(Sheldrick,_1997)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            14177
_diffrn_reflns_theta_full        30.53
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         4.12
_exptl_absorpt_coefficient_mu    4.385
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.51
_refine_diff_density_min         -1.176
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.020(15)
_refine_ls_extinction_coef       0.0058(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         8932
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_gt           0.0709
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.202
_reflns_number_gt                5989
_reflns_number_total             8932
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000064a_1.cif
_cod_data_source_block           Compound2
_cod_database_code               4321002
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z+1/4'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, -z+3/4'
'y, x, -z'
'y+1/2, -x+1/2, z+1/4'
'-y+1/2, x+1/2, z+3/4'
'-y, -x, -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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
_atom_site_disorder_assembly
Re Re 0.78106(3) 0.84660(3) 0.035379(17) 0.04547(18) Uani 1 d . . .
Cl1 Cl 0.6492(2) 0.8641(2) 0.09449(11) 0.0561(7) Uani 1 d . . .
Cl12 Cl 0.70799(17) 0.70799(17) 0 0.0522(9) Uani 1 d S . .
Cl2 Cl 0.8621(6) 0.9646(5) 0.0700(4) 0.084(3) Uani 0.5 d P . .
P1 P 0.8585(2) 0.76551(19) 0.10370(11) 0.0471(6) Uani 1 d . . .
P2 P 0.7030(2) 0.9590(2) -0.01368(12) 0.0492(7) Uani 1 d . . .
N N 0.943(2) 0.9759(17) 0.0344(17) 0.135(15) Uani 0.5 d P . .
C1 C 0.8777(18) 0.9272(16) 0.0370(10) 0.055(6) Uani 0.5 d P . .
C1B C 0.7466(7) 0.9702(7) -0.0788(4) 0.044(2) Uani 1 d . . .
H1B1 H 0.7043 1.0014 -0.1002 0.052 Uiso 1 calc R . .
H1B2 H 0.8016 1.0034 -0.0785 0.052 Uiso 1 calc R . .
C2 C 0.9943(12) 1.0522(11) 0.0455(6) 0.086(9) Uiso 0.5 d PG . .
C3 C 0.9820(11) 1.0989(11) 0.0908(5) 0.133(16) Uiso 0.5 d PG . .
C4 C 1.0344(12) 1.1723(11) 0.1015(5) 0.069(7) Uiso 0.5 d PG . .
H4 H 1.0261 1.2035 0.1318 0.082 Uiso 0.5 calc PR . .
C5 C 1.0991(13) 1.1991(12) 0.0670(7) 0.101(11) Uiso 0.5 d PG . .
H5 H 1.1341 1.2482 0.0742 0.121 Uiso 0.5 calc PR . .
C6 C 1.1114(11) 1.1525(12) 0.0217(6) 0.089(9) Uiso 0.5 d PG . .
H6 H 1.1547 1.1704 -0.0013 0.107 Uiso 0.5 calc PR . .
C7 C 1.0590(11) 1.0790(11) 0.0110(5) 0.055(6) Uiso 0.5 d PG . .
C8 C 0.9028(15) 1.0949(18) 0.1296(8) 0.100(11) Uiso 0.5 d PG . .
H8A H 0.8484 1.1066 0.1118 0.15 Uiso 0.5 calc PR . .
H8B H 0.9114 1.1386 0.1558 0.15 Uiso 0.5 calc PR . .
H8C H 0.9003 1.0371 0.1448 0.15 Uiso 0.5 calc PR . .
C9 C 1.0933(18) 1.0300(16) -0.0402(7) 0.101(11) Uiso 0.5 d PG . .
H9A H 1.1526 1.0489 -0.0478 0.151 Uiso 0.5 calc PR . .
H9B H 1.055 1.0449 -0.0683 0.151 Uiso 0.5 calc PR . .
H9C H 1.0926 0.967 -0.0351 0.151 Uiso 0.5 calc PR . .
C111 C 0.8193(8) 0.6559(7) 0.1260(4) 0.050(3) Uani 1 d . . .
C112 C 0.8792(11) 0.5971(9) 0.1480(4) 0.067(4) Uani 1 d . . .
H112 H 0.9394 0.6101 0.1499 0.08 Uiso 1 calc R . .
C113 C 0.8464(18) 0.5205(10) 0.1665(7) 0.102(6) Uani 1 d . . .
H113 H 0.8855 0.4824 0.1831 0.122 Uiso 1 calc R . .
C114 C 0.7596(16) 0.4945(12) 0.1627(7) 0.098(6) Uani 1 d . . .
H114 H 0.7407 0.4406 0.176 0.118 Uiso 1 calc R . .
C115 C 0.6979(12) 0.5542(11) 0.1371(6) 0.087(5) Uani 1 d . . .
H115 H 0.6389 0.5389 0.1321 0.104 Uiso 1 calc R . .
C116 C 0.7308(10) 0.6340(9) 0.1209(5) 0.070(4) Uani 1 d . . .
H116 H 0.6924 0.6746 0.1059 0.084 Uiso 1 calc R . .
C121 C 0.8786(8) 0.8238(8) 0.1647(5) 0.053(3) Uani 1 d . . .
C122 C 0.9583(11) 0.8178(8) 0.1882(6) 0.070(4) Uani 1 d . . .
H122 H 1.003 0.7846 0.1729 0.083 Uiso 1 calc R . .
C123 C 0.9752(11) 0.8594(12) 0.2342(7) 0.099(7) Uani 1 d . . .
H123 H 1.0307 0.8556 0.2495 0.118 Uiso 1 calc R . .
C124 C 0.9059(12) 0.9082(13) 0.2575(6) 0.093(5) Uani 1 d . . .
H124 H 0.9153 0.9345 0.2892 0.112 Uiso 1 calc R . .
C125 C 0.8256(12) 0.9172(14) 0.2341(7) 0.104(7) Uani 1 d . . .
H125 H 0.7799 0.9509 0.2479 0.125 Uiso 1 calc R . .
C126 C 0.8177(12) 0.8723(14) 0.1884(6) 0.098(6) Uani 1 d . . .
H126 H 0.763 0.8766 0.1721 0.118 Uiso 1 calc R . .
C211 C 0.5857(8) 0.9571(8) -0.0255(4) 0.054(3) Uani 1 d . . .
C212 C 0.5377(8) 0.8792(10) -0.0203(5) 0.066(4) Uani 1 d . . .
H212 H 0.5671 0.8299 -0.0073 0.079 Uiso 1 calc R . .
C213 C 0.4468(9) 0.8695(13) -0.0333(7) 0.086(5) Uani 1 d . . .
H213 H 0.4168 0.8163 -0.0287 0.104 Uiso 1 calc R . .
C214 C 0.4051(11) 0.9437(15) -0.0533(6) 0.091(6) Uani 1 d . . .
H214 H 0.345 0.9415 -0.0611 0.109 Uiso 1 calc R . .
C215 C 0.4522(8) 1.0208(12) -0.0618(7) 0.088(6) Uani 1 d . . .
H215 H 0.4254 1.0692 -0.0774 0.106 Uiso 1 calc R . .
C216 C 0.5437(9) 1.0248(12) -0.0459(6) 0.083(5) Uani 1 d . . .
H216 H 0.5745 1.0776 -0.0504 0.1 Uiso 1 calc R . .
C221 C 0.7180(12) 1.0702(8) 0.0121(5) 0.068(4) Uani 1 d . . .
C222 C 0.7740(10) 1.1294(8) -0.0047(6) 0.071(4) Uani 1 d . . .
H222 H 0.8032 1.115 -0.0349 0.085 Uiso 1 calc R . .
C223 C 0.7961(16) 1.2126(11) 0.0170(7) 0.105(6) Uani 1 d . . .
H223 H 0.8382 1.2518 0.0042 0.127 Uiso 1 calc R . .
C224 C 0.7417(15) 1.2271(11) 0.0630(8) 0.105(7) Uani 1 d . . .
H224 H 0.7549 1.2763 0.083 0.126 Uiso 1 calc R . .
C225 C 0.681(2) 1.1802(13) 0.0770(10) 0.150(12) Uani 1 d . . .
H225 H 0.6447 1.1999 0.1033 0.18 Uiso 1 calc R . .
C226 C 0.6628(18) 1.0892(10) 0.0527(7) 0.120(8) Uani 1 d . . .
H226 H 0.6189 1.0509 0.0642 0.143 Uiso 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 0 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.231 '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
C1 Re Re 87.9(8) . 5 ?
C1 Re Cl2 26.3(8) . . ?
Re Re Cl2 114.2(3) 5 . ?
C1 Re P2 86.4(7) . . ?
Re Re P2 94.76(8) 5 . ?
Cl2 Re P2 85.80(19) . . ?
C1 Re P1 86.4(7) . . ?
Re Re P1 99.49(7) 5 . ?
Cl2 Re P1 81.34(19) . . ?
P2 Re P1 163.78(10) . . ?
C1 Re Cl1 121.5(8) . . ?
Re Re Cl1 150.00(7) 5 . ?
Cl2 Re Cl1 95.5(3) . . ?
P2 Re Cl1 82.46(10) . . ?
P1 Re Cl1 88.95(10) . . ?
C1 Re Cl12 150.3(8) . . ?
Re Re Cl12 62.82(4) 5 . ?
Cl2 Re Cl12 173.65(19) . . ?
P2 Re Cl12 99.90(7) . . ?
P1 Re Cl12 93.51(7) . . ?
Cl1 Re Cl12 88.11(8) . . ?
Re Cl12 Re 54.36(8) . 5 ?
C1B P1 C121 103.3(6) 5 . ?
C1B P1 C111 105.5(5) 5 . ?
C121 P1 C111 101.9(5) . . ?
C1B P1 Re 104.9(3) 5 . ?
C121 P1 Re 117.9(4) . . ?
C111 P1 Re 121.4(4) . . ?
C211 P2 C221 101.6(7) . . ?
C211 P2 C1B 101.2(5) . . ?
C221 P2 C1B 102.4(6) . . ?
C211 P2 Re 123.8(4) . . ?
C221 P2 Re 112.7(5) . . ?
C1B P2 Re 112.4(3) . . ?
C1 N C2 156(4) . . ?
N C1 Re 175(3) . . ?
P1 C1B P2 107.5(5) 5 . ?
C3 C2 C7 120.0(15) . . ?
C3 C2 N 121(2) . . ?
C7 C2 N 119(2) . . ?
C4 C3 C2 120.0(14) . . ?
C4 C3 C8 109.4(15) . . ?
C2 C3 C8 129.3(16) . . ?
C3 C4 C5 120.0(14) . . ?
C4 C5 C6 120.0(16) . . ?
C7 C6 C5 120.0(15) . . ?
C6 C7 C2 120.0(14) . . ?
C6 C7 C9 110.6(15) . . ?
C2 C7 C9 129.1(16) . . ?
C116 C111 C112 121.0(12) . . ?
C116 C111 P1 119.5(10) . . ?
C112 C111 P1 119.5(10) . . ?
C113 C112 C111 117.2(17) . . ?
C112 C113 C114 124.8(19) . . ?
C113 C114 C115 117.9(15) . . ?
C116 C115 C114 117.0(16) . . ?
C115 C116 C111 122.0(15) . . ?
C126 C121 C122 116.2(12) . . ?
C126 C121 P1 123.4(10) . . ?
C122 C121 P1 120.3(10) . . ?
C121 C122 C123 121.9(14) . . ?
C122 C123 C124 118.3(13) . . ?
C125 C124 C123 121.0(14) . . ?
C124 C125 C126 114.7(15) . . ?
C121 C126 C125 127.9(15) . . ?
C216 C211 C212 116.6(13) . . ?
C216 C211 P2 122.1(11) . . ?
C212 C211 P2 120.7(10) . . ?
C211 C212 C213 124.5(14) . . ?
C214 C213 C212 116.5(16) . . ?
C215 C214 C213 120.4(15) . . ?
C214 C215 C216 118.8(14) . . ?
C211 C216 C215 123.0(16) . . ?
C222 C221 C226 120.5(14) . . ?
C222 C221 P2 125.9(11) . . ?
C226 C221 P2 113.6(12) . . ?
C221 C222 C223 128.6(16) . . ?
C222 C223 C224 109.1(16) . . ?
C225 C224 C223 125.5(19) . . ?
C224 C225 C226 122(2) . . ?
C221 C226 C225 113.3(19) . . ?
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
Re C1 1.90(3) . ?
Re Re 2.3195(9) 5 ?
Re Cl2 2.342(7) . ?
Re P2 2.431(3) . ?
Re P1 2.461(3) . ?
Re Cl1 2.533(3) . ?
Re Cl12 2.539(3) . ?
Cl12 Re 2.539(3) 5 ?
P1 C1B 1.829(11) 5 ?
P1 C121 1.848(12) . ?
P1 C111 1.850(11) . ?
P2 C211 1.797(13) . ?
P2 C221 1.823(12) . ?
P2 C1B 1.834(12) . ?
N C1 1.23(4) . ?
N C2 1.42(3) . ?
C1B P1 1.829(11) 5 ?
C2 C3 1.39(2) . ?
C2 C7 1.39(2) . ?
C3 C4 1.39(2) . ?
C3 C8 1.57(3) . ?
C4 C5 1.39(2) . ?
C5 C6 1.39(2) . ?
C6 C7 1.39(2) . ?
C7 C9 1.61(3) . ?
C111 C116 1.383(18) . ?
C111 C112 1.392(19) . ?
C112 C113 1.35(2) . ?
C113 C114 1.37(3) . ?
C114 C115 1.46(3) . ?
C115 C116 1.370(19) . ?
C121 C126 1.33(2) . ?
C121 C122 1.353(18) . ?
C122 C123 1.38(2) . ?
C123 C124 1.42(2) . ?
C124 C125 1.36(2) . ?
C125 C126 1.38(2) . ?
C211 C216 1.315(19) . ?
C211 C212 1.387(19) . ?
C212 C213 1.422(19) . ?
C213 C214 1.39(3) . ?
C214 C215 1.38(2) . ?
C215 C216 1.44(2) . ?
C221 C222 1.305(19) . ?
C221 C226 1.38(2) . ?
C222 C223 1.42(2) . ?
C223 C224 1.47(3) . ?
C224 C225 1.21(3) . ?
C225 C226 1.54(2) . ?
