#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:32:26 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179185 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/31/4313149.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_4313149
loop_
_publ_author_name
'Roberta Visentin'
'Raffaella Rossin'
'Maria Cecilia Giron'
'Alessandro Dolmella'
'Giuliano Bandoli'
'Ulderico Mazzi'
_publ_section_title
;
 Synthesis and Characterization of Rhenium(V) Oxo Complexes with
 N-[N-(3-Diphenylphosphinopropionyl)glycyl]cysteine Methyl Ester. X-ray
 Crystal Structure of {ReO[Ph2P(CH2)2C(O)-Gly-Cys-OMe(P,N,N,S)]}
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              950
_journal_page_last               959
_journal_paper_doi               10.1021/ic025859r
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C21 H23 N2 O5 P Re S'
_chemical_formula_weight         632.64
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.48(3)
_cell_angle_beta                 109.06(3)
_cell_angle_gamma                102.81(3)
_cell_formula_units_Z            2
_cell_length_a                   9.828(2)
_cell_length_b                   11.163(2)
_cell_length_c                   11.641(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.3
_cell_measurement_theta_min      7.7
_cell_volume                     1085.7(6)
_computing_cell_refinement       'P3/P4-PC vers.4.27 (Nicolet, 1991)'
_computing_data_collection       'P3/P4-PC vers.4.27 (Nicolet, 1991)'
_computing_data_reduction        'P3-P4-PC vers.4.27 (Nicolet, 1991)'
_computing_molecular_graphics    'SHELXTL NT vers.5.10 (Sheldrick, 1999)'
_computing_publication_material  'SHELXTL NT vers.5.10 (Sheldrick, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL NT vers.5.10 (Sheldrick, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Nicolet Siemens R3m/V'
_diffrn_measurement_method       theta-2theta
_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  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4966
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         3.33
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count 150
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    5.803
_exptl_absorpt_correction_T_max  0.703
_exptl_absorpt_correction_T_min  0.638
_exptl_absorpt_correction_type   'psi-scans method'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prisms'
_exptl_crystal_F_000             618
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.561
_refine_diff_density_min         -2.146
_refine_diff_density_rms         0.226
_refine_ls_extinction_coef       0.0000(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          1.303
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0949P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1175
_reflns_number_gt                4142
_reflns_number_total             4966
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025859r_s1.cif
_cod_data_source_block           gb8
_cod_original_cell_volume        1085.7(4)
_cod_database_code               4313149
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
Re Re 0.66938(3) 0.76350(3) 0.82461(3) 0.03241(15) Uani 1 1 d . . .
S S 0.7744(3) 0.6655(2) 0.6943(2) 0.0420(5) Uani 1 1 d . . .
P P 0.5528(2) 0.8334(2) 0.64647(19) 0.0328(4) Uani 1 1 d . . .
O1 O 0.5167(7) 0.6558(6) 0.8211(7) 0.0448(14) Uani 1 1 d . . .
O2 O 0.7081(9) 1.1399(7) 1.0632(7) 0.0560(17) Uani 1 1 d . . .
O3 O 1.0306(8) 0.8790(7) 1.1788(7) 0.0584(18) Uani 1 1 d . . .
O4 O 0.7823(10) 0.5683(7) 1.0424(8) 0.0591(18) Uani 1 1 d . . .
O5 O 0.8162(10) 0.4318(7) 0.8826(7) 0.0610(18) Uani 1 1 d . . .
N1 N 0.7336(8) 0.9500(7) 0.9593(7) 0.0372(14) Uani 1 1 d . . .
N2 N 0.8553(7) 0.7706(6) 0.9641(6) 0.0327(13) Uani 1 1 d . . .
C1 C 0.5903(11) 1.0111(9) 0.7192(9) 0.0429(19) Uani 1 1 d . . .
H1A H 0.6976 1.0606 0.7465 0.051 Uiso 1 1 calc R . .
H1B H 0.5285 1.0388 0.6550 0.051 Uiso 1 1 calc R . .
C2 C 0.5502(10) 1.0396(9) 0.8390(9) 0.0417(18) Uani 1 1 d . . .
H2A H 0.5319 1.1234 0.8571 0.050 Uiso 1 1 calc R . .
H2B H 0.4555 0.9703 0.8166 0.050 Uiso 1 1 calc R . .
C3 C 0.6704(9) 1.0466(8) 0.9611(8) 0.0366(16) Uani 1 1 d . . .
C4 C 0.8508(11) 0.9758(9) 1.0897(8) 0.0421(18) Uani 1 1 d . . .
H4A H 0.8039 0.9790 1.1515 0.051 Uiso 1 1 calc R . .
H4B H 0.9300 1.0617 1.1218 0.051 Uiso 1 1 calc R . .
C5 C 0.9219(10) 0.8702(9) 1.0832(8) 0.0407(18) Uani 1 1 d . . .
C6 C 0.9199(9) 0.6644(8) 0.9394(8) 0.0366(16) Uani 1 1 d . . .
H6A H 1.0247 0.6974 1.0078 0.044 Uiso 1 1 calc R . .
C7 C 0.9299(10) 0.6374(9) 0.8084(9) 0.0415(18) Uani 1 1 d . . .
H7A H 0.9243 0.5459 0.7712 0.050 Uiso 1 1 calc R . .
H7B H 1.0277 0.6954 0.8212 0.050 Uiso 1 1 calc R . .
C8 C 0.8321(11) 0.5409(9) 0.9470(9) 0.0417(19) Uani 1 1 d . . .
C9 C 0.7078(14) 0.4559(11) 1.0645(12) 0.061(3) Uani 1 1 d . . .
H9A H 0.6767 0.4863 1.1343 0.092 Uiso 1 1 calc R . .
H9B H 0.7778 0.4103 1.0885 0.092 Uiso 1 1 calc R . .
H9C H 0.6192 0.3961 0.9854 0.092 Uiso 1 1 calc R . .
C10 C 0.3457(9) 0.7611(8) 0.5682(8) 0.0374(16) Uani 1 1 d . . .
C11 C 0.2622(12) 0.7191(14) 0.6331(11) 0.066(3) Uani 1 1 d . . .
H11 H 0.3131 0.7195 0.7161 0.079 Uiso 1 1 calc R . .
C12 C 0.1050(12) 0.677(2) 0.5768(12) 0.100(6) Uani 1 1 d . . .
H12 H 0.0504 0.6465 0.6210 0.120 Uiso 1 1 calc R . .
C13 C 0.0254(13) 0.6787(14) 0.4526(11) 0.069(3) Uani 1 1 d . . .
H13 H -0.0811 0.6528 0.4157 0.082 Uiso 1 1 calc R . .
C14 C 0.1076(10) 0.7191(10) 0.3882(9) 0.049(2) Uani 1 1 d . . .
H14 H 0.0569 0.7184 0.3050 0.059 Uiso 1 1 calc R . .
C15 C 0.2661(10) 0.7614(9) 0.4455(9) 0.047(2) Uani 1 1 d . . .
H15 H 0.3207 0.7906 0.4009 0.056 Uiso 1 1 calc R . .
C16 C 0.6130(9) 0.8079(8) 0.5135(8) 0.0367(16) Uani 1 1 d . . .
C17 C 0.5478(11) 0.6887(9) 0.4065(9) 0.048(2) Uani 1 1 d . . .
H17 H 0.4739 0.6183 0.4039 0.058 Uiso 1 1 calc R . .
C18 C 0.5910(13) 0.6726(10) 0.3030(10) 0.054(2) Uani 1 1 d . . .
H18 H 0.5436 0.5918 0.2307 0.065 Uiso 1 1 calc R . .
C19 C 0.7032(12) 0.7737(10) 0.3044(10) 0.051(2) Uani 1 1 d . . .
H19 H 0.7313 0.7618 0.2341 0.061 Uiso 1 1 calc R . .
C20 C 0.7726(11) 0.8927(11) 0.4131(10) 0.052(2) Uani 1 1 d . . .
H20 H 0.8485 0.9621 0.4166 0.063 Uiso 1 1 calc R . .
C21 C 0.7293(10) 0.9088(9) 0.5164(9) 0.0454(19) Uani 1 1 d . . .
H21 H 0.7786 0.9886 0.5898 0.055 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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
O1 Re N2 107.8(3) . . ?
O1 Re N1 112.7(3) . . ?
N2 Re N1 79.3(3) . . ?
O1 Re S 113.5(2) . . ?
N2 Re S 81.6(2) . . ?
N1 Re S 133.4(2) . . ?
O1 Re P 102.8(2) . . ?
N2 Re P 149.4(2) . . ?
N1 Re P 90.46(19) . . ?
S Re P 85.06(7) . . ?
C7 S Re 103.1(3) . . ?
C16 P C10 105.5(4) . . ?
C16 P C1 106.5(4) . . ?
C10 P C1 103.7(4) . . ?
C16 P Re 118.9(3) . . ?
C10 P Re 113.3(3) . . ?
C1 P Re 107.7(3) . . ?
C8 O4 C9 116.2(8) . . ?
C3 N1 C4 112.8(7) . . ?
C3 N1 Re 132.1(6) . . ?
C4 N1 Re 113.8(5) . . ?
C5 N2 C6 119.0(7) . . ?
C5 N2 Re 120.8(5) . . ?
C6 N2 Re 120.2(5) . . ?
C2 C1 P 108.6(6) . . ?
C3 C2 C1 114.5(7) . . ?
O2 C3 N1 120.7(8) . . ?
O2 C3 C2 118.1(7) . . ?
N1 C3 C2 121.1(7) . . ?
N1 C4 C5 111.3(7) . . ?
O3 C5 N2 125.9(8) . . ?
O3 C5 C4 121.5(8) . . ?
N2 C5 C4 112.7(7) . . ?
N2 C6 C8 112.6(7) . . ?
N2 C6 C7 108.8(6) . . ?
C8 C6 C7 112.2(7) . . ?
C6 C7 S 110.8(5) . . ?
O5 C8 O4 123.1(9) . . ?
O5 C8 C6 124.4(8) . . ?
O4 C8 C6 112.3(7) . . ?
C11 C10 C15 118.1(8) . . ?
C11 C10 P 121.8(7) . . ?
C15 C10 P 119.7(7) . . ?
C12 C11 C10 120.8(10) . . ?
C11 C12 C13 120.6(11) . . ?
C14 C13 C12 118.6(10) . . ?
C13 C14 C15 120.4(9) . . ?
C14 C15 C10 121.5(9) . . ?
C17 C16 C21 117.7(8) . . ?
C17 C16 P 121.4(7) . . ?
C21 C16 P 120.9(6) . . ?
C16 C17 C18 120.7(9) . . ?
C17 C18 C19 121.6(9) . . ?
C20 C19 C18 118.2(9) . . ?
C21 C20 C19 120.1(9) . . ?
C20 C21 C16 121.6(9) . . ?
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 O1 1.682(5) . ?
Re N2 1.976(6) . ?
Re N1 2.027(7) . ?
Re S 2.268(2) . ?
Re P 2.446(2) . ?
S C7 1.823(9) . ?
P C16 1.803(8) . ?
P C10 1.808(8) . ?
P C1 1.819(9) . ?
O2 C3 1.214(10) . ?
O3 C5 1.227(10) . ?
O4 C8 1.341(11) . ?
O4 C9 1.440(12) . ?
O5 C8 1.179(11) . ?
N1 C3 1.357(10) . ?
N1 C4 1.476(10) . ?
N2 C5 1.340(10) . ?
N2 C6 1.467(10) . ?
C1 C2 1.537(12) . ?
C2 C3 1.490(12) . ?
C4 C5 1.495(12) . ?
C6 C8 1.498(12) . ?
C6 C7 1.509(12) . ?
C10 C11 1.378(13) . ?
C10 C15 1.388(12) . ?
C11 C12 1.371(14) . ?
C12 C13 1.410(16) . ?
C13 C14 1.359(15) . ?
C14 C15 1.382(13) . ?
C16 C17 1.376(12) . ?
C16 C21 1.399(12) . ?
C17 C18 1.382(13) . ?
C18 C19 1.385(14) . ?
C19 C20 1.383(15) . ?
C20 C21 1.380(13) . ?
