#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:40:51 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179802 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/98/7009877.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_7009877
loop_
_publ_author_name
'Carvalho, M. Fernanda N. N.'
'Galvão, Adelino M.'
'Pombeiro, Armando J. L.'
_publ_section_title
;
 Proton addition and hydrogen-bond formation in reactions of the
 dicyano-complex [NBu4][trans-Re(CN)2(dppe)2] with protic reagents
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3393
_journal_paper_doi               10.1039/b004189k
_journal_year                    2000
_chemical_formula_sum            'C56 H56 N2 O2 P4 Re'
_chemical_formula_weight         1099.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 107.780(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.474(3)
_cell_length_b                   18.692(2)
_cell_length_c                   10.155(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2435.4(9)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1272
_diffrn_reflns_av_sigmaI/netI    0.1723
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4524
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    2.531
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_F_000             1114
_refine_diff_density_max         1.572
_refine_diff_density_min         -1.364
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.173
_refine_ls_goodness_of_fit_obs   1.144
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         4263
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.176
_refine_ls_restrained_S_obs      1.144
_refine_ls_R_factor_all          0.1796
_refine_ls_R_factor_obs          0.0803
_refine_ls_shift/esd_max         -0.030
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0001P)²+21.4897P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1690
_refine_ls_wR_factor_obs         0.1172
_reflns_number_observed          2291
_reflns_number_total             4266
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b004189k.txt
_cod_data_source_block           Complex5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+21.4897P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+21.4897P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               7009877
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Re Re 1.0000 1.0000 0.5000 0.0261(2) Uani 1 d S .
P1 P 0.8341(3) 0.9899(3) 0.5482(4) 0.0321(11) Uani 1 d . .
P2 P 1.0592(3) 0.9322(2) 0.7124(5) 0.0313(10) Uani 1 d . .
C22 C 1.1797(14) 0.9554(9) 0.8430(19) 0.040(5) Uani 1 d . .
C11 C 0.8579(12) 0.9365(9) 0.7085(16) 0.038(4) Uani 1 d . .
H11A H 0.8069(12) 0.9496(9) 0.7541(16) 0.046 Uiso 1 calc R .
H11B H 0.8484(12) 0.8863(9) 0.6844(16) 0.046 Uiso 1 calc R .
C21 C 0.9650(12) 0.9474(9) 0.8070(17) 0.040(4) Uani 1 d . .
H21A H 0.9774(12) 0.9141(9) 0.8836(17) 0.048 Uiso 1 calc R .
H21B H 0.9720(12) 0.9957(9) 0.8437(17) 0.048 Uiso 1 calc R .
C224 C 1.3709(14) 0.9927(17) 1.0362(17) 0.067(7) Uani 1 d . .
H224 H 1.4341(14) 1.0059(17) 1.0997(17) 0.081 Uiso 1 calc R .
C222 C 1.1944(15) 1.0187(12) 0.9164(18) 0.064(8) Uani 1 d . .
H222 H 1.1394(15) 1.0511(12) 0.8986(18) 0.076 Uiso 1 calc R .
C12 C 0.7210(13) 0.9453(9) 0.4376(21) 0.048(5) Uani 1 d . .
C122 C 0.7270(14) 0.8993(11) 0.3382(19) 0.057(6) Uani 1 d . .
H122 H 0.7905(14) 0.8918(11) 0.3220(19) 0.068 Uiso 1 calc R .
C225 C 1.3625(14) 0.9298(12) 0.9645(19) 0.066(6) Uani 1 d . .
H225 H 1.4196(14) 0.8995(12) 0.9809(19) 0.079 Uiso 1 calc R .
C126 C 0.6223(14) 0.9531(10) 0.4615(23) 0.062(6) Uani 1 d . .
H126 H 0.6167(14) 0.9830(10) 0.5320(23) 0.075 Uiso 1 calc R .
C125 C 0.5348(15) 0.9167(10) 0.3815(23) 0.063(6) Uani 1 d . .
H125 H 0.4707(15) 0.9244(10) 0.3958(23) 0.075 Uiso 1 calc R .
C226 C 1.2689(14) 0.9113(10) 0.8674(19) 0.052(5) Uani 1 d . .
H226 H 1.2646(14) 0.8691(10) 0.8174(19) 0.062 Uiso 1 calc R .
C223 C 1.2854(15) 1.0357(10) 1.0133(19) 0.055(5) Uani 1 d . .
H223 H 1.2897(15) 1.0773(10) 1.0650(19) 0.066 Uiso 1 calc R .
C123 C 0.6387(16) 0.8630(12) 0.2597(19) 0.065(6) Uani 1 d . .
H123 H 0.6448(16) 0.8330(12) 0.1896(19) 0.078 Uiso 1 calc R .
C124 C 0.5422(15) 0.8690(11) 0.2802(24) 0.066(6) Uani 1 d . .
H124 H 0.4851(15) 0.8425(11) 0.2288(24) 0.079 Uiso 1 calc R .
C23 C 1.0700(14) 0.8345(9) 0.7117(20) 0.037(5) Uani 1 d . .
C13 C 0.7786(13) 1.0738(9) 0.5898(19) 0.041(4) Uani 1 d . .
C232 C 1.0979(14) 0.7989(9) 0.6037(19) 0.047(5) Uani 1 d . .
H232 H 1.1047(14) 0.8243(9) 0.5282(19) 0.056 Uiso 1 calc R .
C132 C 0.7165(16) 1.1118(10) 0.4793(25) 0.063(6) Uani 1 d . .
H132 H 0.7038(16) 1.0956(10) 0.3891(25) 0.076 Uiso 1 calc R .
C236 C 1.0582(16) 0.7941(9) 0.8192(21) 0.060(6) Uani 1 d . .
H236 H 1.0394(16) 0.8163(9) 0.8900(21) 0.072 Uiso 1 calc R .
C234 C 1.0979(17) 0.6878(11) 0.7207(20) 0.063(6) Uani 1 d . .
H234 H 1.1037(17) 0.6382(11) 0.7207(20) 0.075 Uiso 1 calc R .
C233 C 1.1140(16) 0.7276(11) 0.6135(21) 0.059(5) Uani 1 d . .
H233 H 1.1365(16) 0.7045(11) 0.5467(21) 0.071 Uiso 1 calc R .
C235 C 1.0741(16) 0.7208(11) 0.8233(20) 0.062(6) Uani 1 d . .
H235 H 1.0682(16) 0.6945(11) 0.8982(20) 0.075 Uiso 1 calc R .
C133 C 0.6722(15) 1.1772(11) 0.5080(27) 0.068(7) Uani 1 d . .
H133 H 0.6293(15) 1.2042(11) 0.4361(27) 0.082 Uiso 1 calc R .
C134 C 0.6938(16) 1.2004(12) 0.6452(27) 0.074(7) Uani 1 d . .
H134 H 0.6661(16) 1.2429(12) 0.6662(27) 0.088 Uiso 1 calc R .
C136 C 0.7946(17) 1.0954(10) 0.7187(25) 0.069(7) Uani 1 d . .
H136 H 0.8328(17) 1.0672(10) 0.7921(25) 0.083 Uiso 1 calc R .
C135 C 0.7544(18) 1.1600(11) 0.7433(27) 0.074(7) Uani 1 d . .
H135 H 0.7710(18) 1.1759(11) 0.8342(27) 0.089 Uiso 1 calc R .
N1 N 1.0360(13) 1.1372(10) 0.7012(18) 0.055(5) Uani 1 d . .
C1 C 1.0207(13) 1.0896(10) 0.6225(16) 0.040(5) Uani 1 d . .
O2S O 1.0417(17) 1.2179(13) 0.9328(20) 0.141(9) Uani 1 d . .
H2S H 1.0313(17) 1.1873(13) 0.8722(20) 0.038(58) Uiso 1 calc R .
C2S C 1.1421(21) 1.2202(13) 1.0014(30) 0.102(10) Uani 1 d . .
H2SA H 1.1818(21) 1.2105(13) 0.9394(30) 0.122 Uiso 1 calc R .
H2SB H 1.1579(21) 1.1850(13) 1.0737(30) 0.122 Uiso 1 calc R .
H2SC H 1.1596(21) 1.2669(13) 1.0411(30) 0.122 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 0.0020 0.0020 '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'
P P 0.0900 0.0950 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.5980 7.2320 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0080 0.0060 '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 C1 180.000(4) 3_776 . ?
C1 Re P2 93.4(4) 3_776 . ?
C1 Re P2 86.6(4) . . ?
C1 Re P2 86.6(4) 3_776 3_776 ?
C1 Re P2 93.4(4) . 3_776 ?
P2 Re P2 180.0 . 3_776 ?
C1 Re P1 84.5(5) 3_776 3_776 ?
C1 Re P1 95.5(5) . 3_776 ?
P2 Re P1 98.42(15) . 3_776 ?
P2 Re P1 81.58(14) 3_776 3_776 ?
C1 Re P1 95.5(5) 3_776 . ?
C1 Re P1 84.5(5) . . ?
P2 Re P1 81.58(14) . . ?
P2 Re P1 98.42(15) 3_776 . ?
P1 Re P1 180.0 3_776 . ?
C12 P1 C13 102.3(8) . . ?
C12 P1 C11 100.7(9) . . ?
C13 P1 C11 103.3(8) . . ?
C12 P1 Re 124.4(6) . . ?
C13 P1 Re 116.2(6) . . ?
C11 P1 Re 107.1(5) . . ?
C22 P2 C23 100.8(8) . . ?
C22 P2 C21 100.9(8) . . ?
C23 P2 C21 103.0(8) . . ?
C22 P2 Re 120.4(6) . . ?
C23 P2 Re 121.6(7) . . ?
C21 P2 Re 107.1(5) . . ?
C222 C22 C226 115.6(18) . . ?
C222 C22 P2 123.4(15) . . ?
C226 C22 P2 120.8(14) . . ?
C21 C11 P1 112.8(11) . . ?
C11 C21 P2 108.0(11) . . ?
C223 C224 C225 119.1(18) . . ?
C223 C222 C22 122.8(20) . . ?
C122 C12 C126 117.7(17) . . ?
C122 C12 P1 122.1(13) . . ?
C126 C12 P1 120.0(15) . . ?
C12 C122 C123 120.3(18) . . ?
C224 C225 C226 120.2(19) . . ?
C125 C126 C12 121.2(20) . . ?
C124 C125 C126 120.5(19) . . ?
C225 C226 C22 121.1(18) . . ?
C222 C223 C224 121.0(20) . . ?
C124 C123 C122 123.6(20) . . ?
C123 C124 C125 116.6(19) . . ?
C236 C23 C232 118.3(16) . . ?
C236 C23 P2 121.0(15) . . ?
C232 C23 P2 120.5(13) . . ?
C136 C13 C132 121.6(19) . . ?
C136 C13 P1 122.2(16) . . ?
C132 C13 P1 116.2(15) . . ?
C233 C232 C23 118.6(17) . . ?
C13 C132 C133 117.6(22) . . ?
C23 C236 C235 120.8(19) . . ?
C235 C234 C233 119.8(19) . . ?
C232 C233 C234 121.9(20) . . ?
C234 C235 C236 120.5(18) . . ?
C134 C133 C132 119.6(21) . . ?
C135 C134 C133 117.8(22) . . ?
C13 C136 C135 119.6(23) . . ?
C134 C135 C136 123.5(24) . . ?
N1 C1 Re 174.7(15) . . ?
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 2.05(2) 3_776 ?
Re C1 2.05(2) . ?
Re P2 2.418(4) . ?
Re P2 2.418(4) 3_776 ?
Re P1 2.437(4) 3_776 ?
Re P1 2.437(4) . ?
P1 C12 1.80(2) . ?
P1 C13 1.84(2) . ?
P1 C11 1.85(2) . ?
P2 C22 1.81(2) . ?
P2 C23 1.83(2) . ?
P2 C21 1.833(14) . ?
C22 C222 1.38(3) . ?
C22 C226 1.42(2) . ?
C11 C21 1.50(2) . ?
C224 C223 1.37(3) . ?
C224 C225 1.37(3) . ?
C222 C223 1.36(2) . ?
C12 C122 1.35(2) . ?
C12 C126 1.43(2) . ?
C122 C123 1.39(2) . ?
C225 C226 1.39(2) . ?
C126 C125 1.39(3) . ?
C125 C124 1.39(3) . ?
C123 C124 1.38(3) . ?
C23 C236 1.38(2) . ?
C23 C232 1.43(2) . ?
C13 C136 1.32(3) . ?
C13 C132 1.38(3) . ?
C232 C233 1.35(2) . ?
C132 C133 1.43(3) . ?
C236 C235 1.39(2) . ?
C234 C235 1.33(3) . ?
C234 C233 1.39(2) . ?
C133 C134 1.40(3) . ?
C134 C135 1.32(3) . ?
C136 C135 1.38(2) . ?
N1 C1 1.17(2) . ?
O2S C2S 1.32(3) . ?
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
C1 Re P1 C12 -25.3(9) 3_776 . . . ?
C1 Re P1 C12 154.7(9) . . . . ?
P2 Re P1 C12 -117.9(8) . . . . ?
P2 Re P1 C12 62.1(8) 3_776 . . . ?
P1 Re P1 C12 -127.7(1000) 3_776 . . . ?
C1 Re P1 C13 -153.9(8) 3_776 . . . ?
C1 Re P1 C13 26.1(8) . . . . ?
P2 Re P1 C13 113.5(7) . . . . ?
P2 Re P1 C13 -66.5(7) 3_776 . . . ?
P1 Re P1 C13 103.7(1000) 3_776 . . . ?
C1 Re P1 C11 91.2(7) 3_776 . . . ?
C1 Re P1 C11 -88.8(7) . . . . ?
P2 Re P1 C11 -1.4(6) . . . . ?
P2 Re P1 C11 178.6(6) 3_776 . . . ?
P1 Re P1 C11 -11.2(1000) 3_776 . . . ?
C1 Re P2 C22 128.5(8) 3_776 . . . ?
C1 Re P2 C22 -51.5(8) . . . . ?
P2 Re P2 C22 0.0(1000) 3_776 . . . ?
P1 Re P2 C22 43.5(7) 3_776 . . . ?
P1 Re P2 C22 -136.5(7) . . . . ?
C1 Re P2 C23 0.4(8) 3_776 . . . ?
C1 Re P2 C23 -179.6(8) . . . . ?
P2 Re P2 C23 0.0(1000) 3_776 . . . ?
P1 Re P2 C23 -84.6(7) 3_776 . . . ?
P1 Re P2 C23 95.4(7) . . . . ?
C1 Re P2 C21 -117.4(8) 3_776 . . . ?
C1 Re P2 C21 62.6(8) . . . . ?
P2 Re P2 C21 0.0(1000) 3_776 . . . ?
P1 Re P2 C21 157.7(6) 3_776 . . . ?
P1 Re P2 C21 -22.3(6) . . . . ?
C23 P2 C22 C222 -157.0(16) . . . . ?
C21 P2 C22 C222 -51.3(17) . . . . ?
Re P2 C22 C222 66.0(17) . . . . ?
C23 P2 C22 C226 28.6(16) . . . . ?
C21 P2 C22 C226 134.2(15) . . . . ?
Re P2 C22 C226 -108.4(14) . . . . ?
C12 P1 C11 C21 163.4(12) . . . . ?
C13 P1 C11 C21 -91.1(12) . . . . ?
Re P1 C11 C21 32.1(13) . . . . ?
P1 C11 C21 P2 -52.4(14) . . . . ?
C22 P2 C21 C11 175.1(12) . . . . ?
C23 P2 C21 C11 -81.0(13) . . . . ?
Re P2 C21 C11 48.4(12) . . . . ?
C226 C22 C222 C223 -4.8(29) . . . . ?
P2 C22 C222 C223 -179.5(16) . . . . ?
C13 P1 C12 C122 151.0(17) . . . . ?
C11 P1 C12 C122 -102.6(18) . . . . ?
Re P1 C12 C122 16.9(21) . . . . ?
C13 P1 C12 C126 -34.6(18) . . . . ?
C11 P1 C12 C126 71.7(17) . . . . ?
Re P1 C12 C126 -168.8(13) . . . . ?
C126 C12 C122 C123 2.1(31) . . . . ?
P1 C12 C122 C123 176.6(16) . . . . ?
C223 C224 C225 C226 1.7(32) . . . . ?
C122 C12 C126 C125 -2.6(31) . . . . ?
P1 C12 C126 C125 -177.1(16) . . . . ?
C12 C126 C125 C124 3.2(32) . . . . ?
C224 C225 C226 C22 -1.8(32) . . . . ?
C222 C22 C226 C225 3.2(27) . . . . ?
P2 C22 C226 C225 178.0(15) . . . . ?
C22 C222 C223 C224 5.0(32) . . . . ?
C225 C224 C223 C222 -3.2(32) . . . . ?
C12 C122 C123 C124 -2.4(35) . . . . ?
C122 C123 C124 C125 2.9(33) . . . . ?
C126 C125 C124 C123 -3.2(31) . . . . ?
C22 P2 C23 C236 72.6(18) . . . . ?
C21 P2 C23 C236 -31.4(18) . . . . ?
Re P2 C23 C236 -151.1(14) . . . . ?
C22 P2 C23 C232 -103.1(16) . . . . ?
C21 P2 C23 C232 152.9(15) . . . . ?
Re P2 C23 C232 33.2(18) . . . . ?
C12 P1 C13 C136 127.0(17) . . . . ?
C11 P1 C13 C136 22.7(18) . . . . ?
Re P1 C13 C136 -94.3(16) . . . . ?
C12 P1 C13 C132 -51.0(16) . . . . ?
C11 P1 C13 C132 -155.3(14) . . . . ?
Re P1 C13 C132 87.7(14) . . . . ?
C236 C23 C232 C233 -1.7(29) . . . . ?
P2 C23 C232 C233 174.2(15) . . . . ?
C136 C13 C132 C133 2.0(28) . . . . ?
P1 C13 C132 C133 180.0(13) . . . . ?
C232 C23 C236 C235 0.7(31) . . . . ?
P2 C23 C236 C235 -175.1(17) . . . . ?
C23 C232 C233 C234 4.1(31) . . . . ?
C235 C234 C233 C232 -5.6(34) . . . . ?
C233 C234 C235 C236 4.5(34) . . . . ?
C23 C236 C235 C234 -2.2(35) . . . . ?
C13 C132 C133 C134 0.6(28) . . . . ?
C132 C133 C134 C135 -0.4(31) . . . . ?
C132 C13 C136 C135 -4.6(31) . . . . ?
P1 C13 C136 C135 177.5(15) . . . . ?
C133 C134 C135 C136 -2.3(35) . . . . ?
C13 C136 C135 C134 4.9(35) . . . . ?
C1 Re C1 N1 11.5(1000) 3_776 . . . ?
P2 Re C1 N1 6.5(173) . . . . ?
P2 Re C1 N1 -173.5(173) 3_776 . . . ?
P1 Re C1 N1 -91.7(174) 3_776 . . . ?
P1 Re C1 N1 88.3(174) . . . . ?
