#------------------------------------------------------------------------------
#$Date: 2016-02-16 21:30:59 +0100 (mar 16 de feb de 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/31/4313104.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_4313104
loop_
_publ_author_name
'Mani Ganesan'
'Keng-Yu Shih'
'Phillip E. Fanwick'
'Richard A. Walton'
_publ_section_title
;
 Complexation of the Triply-Bonded Dirhenium(II) Complex Re2Cl4(μ-dppm)2
 (dppm = Ph2PCH2PPh2) by Up to Three Acetylene Molecules
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1241
_journal_page_last               1247
_journal_paper_doi               10.1021/ic020532b
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C52 H52 Cl3 F6 O P5 Re2'
_chemical_formula_weight         1440.54
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 93.0710(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.9178(3)
_cell_length_b                   14.7997(4)
_cell_length_c                   14.9895(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2861.57(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0614
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11214
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         5.00
_exptl_absorpt_coefficient_mu    4.561
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1404
_refine_diff_density_max         2.780
_refine_diff_density_min         -2.502
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         6959
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0828P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1350
_reflns_number_gt                5200
_reflns_number_total             6959
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020532b_3.cif
_cod_data_source_block           xl
_cod_original_formula_sum        'C52 H6 H46 Cl3 F6 O P5 Re2'
_cod_database_code               4313104
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
Re Re 0.073255(17) 0.153333(16) 0.238527(17) 0.02802(10) Uani 1 1 d . . .
Cl1 Cl 0.05232(12) 0.01682(11) 0.32861(13) 0.0434(4) Uani 1 1 d . . .
Cl11 Cl 0.04073(14) 0.2500 0.36505(15) 0.0278(4) Uani 1 2 d S . .
P1 P -0.12051(12) 0.14655(10) 0.22415(11) 0.0276(3) Uani 1 1 d . . .
P2 P 0.25253(11) 0.14626(11) 0.31188(12) 0.0289(3) Uani 1 1 d . . .
P100 P 0.51236(16) 0.2500 0.02413(16) 0.0324(5) Uani 1 2 d S . .
F1 F 0.5114(3) 0.1427(3) 0.0241(3) 0.0456(11) Uani 1 1 d . . .
F2 F 0.4005(3) 0.2500 0.0687(4) 0.0345(11) Uani 1 2 d S . .
F3 F 0.5683(4) 0.2500 0.1230(4) 0.0510(15) Uani 1 2 d S . .
F4 F 0.4546(4) 0.2500 -0.0729(4) 0.0398(13) Uani 1 2 d S . .
F5 F 0.6233(4) 0.2500 -0.0191(5) 0.0529(16) Uani 1 2 d S . .
O1W O 0.8718(13) 0.2500 0.7171(9) 0.126(5) Uani 1 2 d S . .
C1 C 0.1442(6) 0.0635(5) 0.1456(5) 0.0438(18) Uani 1 1 d . . .
H1 H 0.207(5) 0.044(5) 0.135(5) 0.05(2) Uiso 1 1 d . . .
C2 C 0.0541(6) 0.0655(5) 0.1223(5) 0.0432(18) Uani 1 1 d . . .
H2 H -0.003(7) 0.046(7) 0.091(7) 0.07(3) Uiso 1 1 d . . .
C11 C 0.1471(6) 0.2500 0.1612(6) 0.0320(19) Uani 1 2 d S . .
H11 H 0.2163 0.2500 0.1250 0.12(6) Uiso 1 2 d S . .
C12 C 0.0448(7) 0.2500 0.1358(7) 0.0313(19) Uani 1 2 d S . .
H12 H 0.040(11) 0.2500 0.088(11) 0.09(5) Uiso 1 2 d S . .
C1B C -0.1747(6) 0.2500 0.1739(5) 0.0239(16) Uani 1 2 d S . .
H1B1 H -0.2491 0.2500 0.1797 0.029 Uiso 1 2 calc SR . .
H1B2 H -0.1623 0.2500 0.1107 0.029 Uiso 1 2 calc SR . .
C2B C 0.3256(6) 0.2500 0.2919(6) 0.0328(19) Uani 1 2 d S . .
H2B1 H 0.3884 0.2500 0.3304 0.039 Uiso 1 2 calc SR . .
H2B2 H 0.3461 0.2500 0.2305 0.039 Uiso 1 2 calc SR . .
C111 C -0.1959(5) 0.1341(4) 0.3232(5) 0.0345(15) Uani 1 1 d . . .
C112 C -0.3014(6) 0.1323(10) 0.3100(7) 0.102(5) Uani 1 1 d . . .
H112 H -0.3317 0.1351 0.2524 0.123 Uiso 1 1 calc R . .
C113 C -0.3630(8) 0.1261(15) 0.3825(11) 0.180(11) Uani 1 1 d . . .
H113 H -0.4348 0.1283 0.3731 0.216 Uiso 1 1 calc R . .
C114 C -0.3217(8) 0.1172(9) 0.4654(7) 0.093(4) Uani 1 1 d . . .
H114 H -0.3646 0.1121 0.5131 0.112 Uiso 1 1 calc R . .
C115 C -0.2161(6) 0.1156(5) 0.4804(5) 0.0498(19) Uani 1 1 d . . .
H115 H -0.1868 0.1098 0.5382 0.060 Uiso 1 1 calc R . .
C116 C -0.1547(5) 0.1225(5) 0.4096(5) 0.0367(14) Uani 1 1 d . . .
H116 H -0.0832 0.1194 0.4196 0.044 Uiso 1 1 calc R . .
C121 C -0.1791(5) 0.0570(4) 0.1539(5) 0.0348(15) Uani 1 1 d . . .
C122 C -0.1593(7) -0.0307(5) 0.1805(6) 0.056(2) Uani 1 1 d . . .
H122 H -0.1143 -0.0427 0.2295 0.067 Uiso 1 1 calc R . .
C123 C -0.2087(8) -0.1027(6) 0.1318(7) 0.069(3) Uani 1 1 d . . .
H123 H -0.1965 -0.1621 0.1498 0.083 Uiso 1 1 calc R . .
C124 C -0.2740(6) -0.0855(6) 0.0590(6) 0.058(2) Uani 1 1 d . . .
H124 H -0.3059 -0.1326 0.0269 0.069 Uiso 1 1 calc R . .
C125 C -0.2915(5) 0.0023(6) 0.0342(6) 0.050(2) Uani 1 1 d . . .
H125 H -0.3356 0.0144 -0.0154 0.060 Uiso 1 1 calc R . .
C126 C -0.2454(5) 0.0732(5) 0.0807(5) 0.0415(16) Uani 1 1 d . . .
H126 H -0.2592 0.1322 0.0626 0.050 Uiso 1 1 calc R . .
C211 C 0.2702(5) 0.1314(5) 0.4335(5) 0.0386(16) Uani 1 1 d . . .
C212 C 0.1918(5) 0.1216(5) 0.4909(5) 0.0363(14) Uani 1 1 d . . .
H212 H 0.1234 0.1202 0.4682 0.044 Uiso 1 1 calc R . .
C213 C 0.2126(7) 0.1138(5) 0.5817(5) 0.0498(19) Uani 1 1 d . . .
H213 H 0.1578 0.1086 0.6192 0.060 Uiso 1 1 calc R . .
C214 C 0.3108(9) 0.1134(9) 0.6171(6) 0.085(4) Uani 1 1 d . . .
H214 H 0.3246 0.1079 0.6784 0.103 Uiso 1 1 calc R . .
C215 C 0.3894(9) 0.1215(15) 0.5600(8) 0.175(10) Uani 1 1 d . . .
H215 H 0.4578 0.1212 0.5829 0.210 Uiso 1 1 calc R . .
C216 C 0.3698(7) 0.1297(12) 0.4720(7) 0.125(7) Uani 1 1 d . . .
H216 H 0.4252 0.1344 0.4352 0.150 Uiso 1 1 calc R . .
C221 C 0.3365(4) 0.0584(4) 0.2726(4) 0.0318(14) Uani 1 1 d . . .
C222 C 0.3163(6) -0.0308(6) 0.2967(6) 0.059(2) Uani 1 1 d . . .
H222 H 0.2619 -0.0426 0.3332 0.070 Uiso 1 1 calc R . .
C223 C 0.3748(7) -0.1014(5) 0.2680(7) 0.065(3) Uani 1 1 d . . .
H223 H 0.3623 -0.1597 0.2880 0.077 Uiso 1 1 calc R . .
C224 C 0.4527(6) -0.0862(5) 0.2090(5) 0.0456(17) Uani 1 1 d . . .
H224 H 0.4910 -0.1341 0.1876 0.055 Uiso 1 1 calc R . .
C225 C 0.4715(5) 0.0003(5) 0.1833(5) 0.0410(16) Uani 1 1 d . . .
H225 H 0.5236 0.0111 0.1441 0.049 Uiso 1 1 calc R . .
C226 C 0.4145(5) 0.0732(5) 0.2141(5) 0.0357(14) Uani 1 1 d . . .
H226 H 0.4289 0.1316 0.1954 0.043 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'
Re Re -1.0185 7.2310 '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'
P P 0.1023 0.0942 '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'
O O 0.0106 0.0060 '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'
H H 0.0000 0.0000 '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
C11 Re C12 37.5(3) . . ?
C11 Re C1 81.0(3) . . ?
C12 Re C1 90.6(3) . . ?
C11 Re C2 90.1(3) . . ?
C12 Re C2 79.3(3) . . ?
C1 Re C2 32.0(3) . . ?
C11 Re Cl11 97.60(19) . . ?
C12 Re Cl11 98.0(2) . . ?
C1 Re Cl11 163.9(2) . . ?
C2 Re Cl11 163.5(2) . . ?
C11 Re Cl1 158.54(19) . . ?
C12 Re Cl1 159.4(2) . . ?
C1 Re Cl1 84.9(2) . . ?
C2 Re Cl1 86.4(2) . . ?
Cl11 Re Cl1 91.52(5) . . ?
C11 Re P1 117.5(2) . . ?
C12 Re P1 80.2(2) . . ?
C1 Re P1 112.1(2) . . ?
C2 Re P1 80.6(2) . . ?
Cl11 Re P1 82.93(6) . . ?
Cl1 Re P1 82.83(5) . . ?
C11 Re P2 80.5(2) . . ?
C12 Re P2 117.8(2) . . ?
C1 Re P2 81.0(2) . . ?
C2 Re P2 112.8(2) . . ?
Cl11 Re P2 82.92(6) . . ?
Cl1 Re P2 81.43(5) . . ?
P1 Re P2 158.48(6) . . ?
C11 Re Re 47.11(16) . 4_565 ?
C12 Re Re 47.55(18) . 4_565 ?
C1 Re Re 127.9(2) . 4_565 ?
C2 Re Re 126.7(2) . 4_565 ?
Cl11 Re Re 53.93(3) . 4_565 ?
Cl1 Re Re 145.45(5) . 4_565 ?
P1 Re Re 92.30(4) . 4_565 ?
P2 Re Re 92.39(4) . 4_565 ?
Re Cl11 Re 72.13(6) 4_565 . ?
C111 P1 C1B 102.1(3) . . ?
C111 P1 C121 100.0(3) . . ?
C1B P1 C121 103.4(3) . . ?
C111 P1 Re 120.5(2) . . ?
C1B P1 Re 111.1(2) . . ?
C121 P1 Re 117.3(2) . . ?
C221 P2 C2B 103.0(3) . . ?
C221 P2 C211 101.1(3) . . ?
C2B P2 C211 103.0(4) . . ?
C221 P2 Re 116.2(2) . . ?
C2B P2 Re 111.3(3) . . ?
C211 P2 Re 120.1(2) . . ?
F1 P100 F1 179.2(3) . 4_565 ?
F1 P100 F4 89.79(19) . . ?
F1 P100 F4 89.79(19) 4_565 . ?
F1 P100 F5 90.37(17) . . ?
F1 P100 F5 90.37(17) 4_565 . ?
F4 P100 F5 90.9(3) . . ?
F1 P100 F3 90.20(19) . . ?
F1 P100 F3 90.20(19) 4_565 . ?
F4 P100 F3 178.8(3) . . ?
F5 P100 F3 90.3(3) . . ?
F1 P100 F2 89.63(17) . . ?
F1 P100 F2 89.63(17) 4_565 . ?
F4 P100 F2 89.5(3) . . ?
F5 P100 F2 179.5(3) . . ?
F3 P100 F2 89.2(3) . . ?
H1 C1 C2 148(5) . . ?
H1 C1 Re 138(5) . . ?
C2 C1 Re 74.6(5) . . ?
H2 C2 C1 154(6) . . ?
H2 C2 Re 132(6) . . ?
C1 C2 Re 73.4(5) . . ?
H11 C11 C12 133.3(9) . . ?
H11 C11 Re 134.1(2) . 4_565 ?
C12 C11 Re 72.0(4) . 4_565 ?
H11 C11 Re 134.1(2) . . ?
C12 C11 Re 72.0(4) . . ?
Re C11 Re 85.8(3) 4_565 . ?
H12 C12 C11 108(10) . . ?
H12 C12 Re 137(2) . 4_565 ?
C11 C12 Re 70.6(4) . 4_565 ?
H12 C12 Re 137(2) . . ?
C11 C12 Re 70.6(4) . . ?
Re C12 Re 84.9(4) 4_565 . ?
P1 C1B P1 113.7(4) . 4_565 ?
P2 C2B P2 113.5(5) 4_565 . ?
C112 C111 C116 117.5(7) . . ?
C112 C111 P1 117.1(6) . . ?
C116 C111 P1 125.3(5) . . ?
C111 C112 C113 120.0(10) . . ?
C114 C113 C112 121.3(10) . . ?
C113 C114 C115 120.0(9) . . ?
C116 C115 C114 119.1(8) . . ?
C115 C116 C111 121.9(7) . . ?
C126 C121 C122 119.4(7) . . ?
C126 C121 P1 123.6(5) . . ?
C122 C121 P1 116.8(5) . . ?
C121 C122 C123 119.1(8) . . ?
C124 C123 C122 120.6(9) . . ?
C125 C124 C123 118.7(7) . . ?
C124 C125 C126 121.7(7) . . ?
C121 C126 C125 120.4(7) . . ?
C212 C211 C216 116.0(7) . . ?
C212 C211 P2 125.3(5) . . ?
C216 C211 P2 118.7(6) . . ?
C211 C212 C213 121.1(7) . . ?
C214 C213 C212 121.2(8) . . ?
C213 C214 C215 117.9(8) . . ?
C216 C215 C214 121.2(9) . . ?
C215 C216 C211 122.5(9) . . ?
C226 C221 C222 117.7(6) . . ?
C226 C221 P2 124.0(5) . . ?
C222 C221 P2 118.1(5) . . ?
C223 C222 C221 121.7(7) . . ?
C222 C223 C224 120.3(7) . . ?
C225 C224 C223 118.5(6) . . ?
C224 C225 C226 121.8(7) . . ?
C221 C226 C225 119.9(6) . . ?
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 C11 2.102(6) . ?
Re C12 2.120(7) . ?
Re C1 2.164(7) . ?
Re C2 2.177(7) . ?
Re Cl11 2.4301(18) . ?
Re Cl1 2.4530(17) . ?
Re P1 2.5028(15) . ?
Re P2 2.5120(16) . ?
Re Re 2.8613(5) 4_565 ?
Cl11 Re 2.4301(18) 4_565 ?
P1 C111 1.828(7) . ?
P1 C1B 1.829(5) . ?
P1 C121 1.831(6) . ?
P2 C221 1.812(6) . ?
P2 C2B 1.836(5) . ?
P2 C211 1.839(7) . ?
P100 F1 1.588(4) . ?
P100 F1 1.588(4) 4_565 ?
P100 F4 1.599(6) . ?
P100 F5 1.604(6) . ?
P100 F3 1.613(6) . ?
P100 F2 1.624(5) . ?
C1 H1 0.88(7) . ?
C1 C2 1.198(10) . ?
C2 H2 0.90(9) . ?
C11 H11 1.070(8) . ?
C11 C12 1.356(12) . ?
C11 Re 2.102(6) 4_565 ?
C12 H12 0.72(16) . ?
C12 Re 2.120(7) 4_565 ?
C1B P1 1.829(5) 4_565 ?
C2B P2 1.836(5) 4_565 ?
C111 C112 1.367(10) . ?
C111 C116 1.385(10) . ?
C112 C113 1.383(15) . ?
C113 C114 1.333(18) . ?
C114 C115 1.372(13) . ?
C115 C116 1.362(10) . ?
C121 C126 1.376(9) . ?
C121 C122 1.377(10) . ?
C122 C123 1.423(11) . ?
C123 C124 1.367(13) . ?
C124 C125 1.366(12) . ?
C125 C126 1.377(10) . ?
C211 C212 1.371(9) . ?
C211 C216 1.382(10) . ?
C212 C213 1.377(10) . ?
C213 C214 1.349(13) . ?
C214 C215 1.368(16) . ?
C215 C216 1.335(14) . ?
C221 C226 1.389(8) . ?
C221 C222 1.396(10) . ?
C222 C223 1.372(11) . ?
C223 C224 1.393(12) . ?
C224 C225 1.363(10) . ?
C225 C226 1.399(9) . ?
