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#$Date: 2025-08-21 00:01:10 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301838 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/40/4324059.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_4324059
loop_
_publ_author_name
'V. Sreenivasa Reddy'
'Douglas E. Berning'
'Kattesh Katti'
'Charles L. Barnes'
'Wynn A. Volkert'
'A.R. Kettring'
_publ_contact_author
;
Kattesh V. Katti
Center for Radiological Research and MURR
University of Missouri
Columbia, MO 65211
;
_publ_section_title
;
 Chemistry in Environmentally Benign Media. 3.1 Synthesis and
 Characterization of Rhenium(V) Complexes Derived from Novel Water-Soluble
 (Hydroxymethyl)phosphines. Crystal Structures of
 [Re(O)2{(HOH2C)2PC6H4P(CH2OH)2}2]I and
 [Re(O)2{(HOH2C)2PCH2CH2P(CH2OH)2}2]Cl
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1753
_journal_page_last               1757
_journal_paper_doi               10.1021/ic9510167
_journal_volume                  35
_journal_year                    1996
_chemical_formula_moiety         'C20 H32 O10 P4 Re I '
_chemical_formula_sum            'C20 H32 I O10 P4 Re'
_chemical_formula_weight         869.47
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.0
_cell_angle_beta                 105.929(9)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   23.906(5)
_cell_length_b                   7.0493(6)
_cell_length_c                   17.024(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      15.00
_cell_measurement_theta_min      10.00
_cell_volume                     2758.7(9)
_computing_data_reduction        'NRCVAX DATRD2'
_computing_molecular_graphics    NRCVAX
_computing_publication_material  'NRCVAX TABLES'
_computing_structure_refinement  'NRCVAX LSTSQ'
_computing_structure_solution    'NRCVAX SOLVER'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Nonius CAD-4    '
_diffrn_measurement_method       'Theta/2theta scan b/P/b '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'xray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2554
_diffrn_reflns_theta_max         24.91
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.74
_exptl_absorpt_correction_T_max  0.9939
_exptl_absorpt_correction_T_min  0.6349
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    2.093
_exptl_crystal_F_000             1674.18
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.35
_refine_diff_density_min         -1.04
_refine_ls_goodness_of_fit_obs   1.21
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2280
_refine_ls_R_factor_all          0.019
_refine_ls_R_factor_obs          0.019
_refine_ls_shift/esd_max         0.011
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/(σ²(F)+0.0003F²)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.027
_refine_ls_wR_factor_obs         0.027
_reflns_number_observed          2280
_reflns_number_total             2421
_reflns_observed_criterion       'Inet > 2.0\s(Inet)'
_cod_data_source_file            ic9510167_1.cif
_cod_data_source_block           C20H32O10P4ReI
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/(\s^2^(F)+0.0003F^2^)' 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^(F)+0.0003F^2^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C20 H32 O10 P4 Re I '
_cod_database_code               4324059
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
1/2+x,1/2+y,z
1/2-x,1/2-y,-z
-x,y,1/2-z
x,-y,1/2+z
1/2-x,1/2+y,1/2-z
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_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_calc_flag
_atom_site_refinement_flags
_atom_site_type_symbol
Re 0.75000 0.25000 0.00000 0.01670(12) Uij ? S Re
P1 0.84158(3) 0.29557(12) 0.10771(5) 0.0213(4) Uij ? . P
P2 0.68057(3) 0.36459(10) 0.07213(4) 0.0208(4) Uij ? . P
O1 0.89997(11) 0.1539(4) 0.25653(14) 0.0458(14) Uij ? . O
O2 0.86102(18) 0.6703(4) 0.11214(19) 0.080(3) Uij ? . O
O3 0.74116(11) 0.3523(4) 0.22577(15) 0.0392(14) Uij ? . O
O4 0.72382(12) 0.7154(4) 0.11879(16) 0.0353(14) Uij ? . O
O5 0.74284(8) 0.0189(3) 0.03817(12) 0.0267(10) Uij ? . O
C1 0.85174(13) 0.1151(5) 0.18887(19) 0.0314(16) Uij ? . C
C2 0.85377(13) 0.5229(5) 0.16262(20) 0.0325(16) Uij ? . C
C3 0.69001(18) 0.2708(5) 0.17547(24) 0.0314(19) Uij ? . C
C4 0.67086(14) 0.6228(4) 0.07953(20) 0.0307(16) Uij ? . C
C5 0.90283(15) 0.2731(4) 0.06434(22) 0.0258(16) Uij ? . C
C6 0.95919(13) 0.3198(5) 0.10913(20) 0.0325(17) Uij ? . C
C7 1.00481(15) 0.3028(6) 0.0736(3) 0.0392(20) Uij ? . C
C8 0.50514(20) 0.2590(5) 0.0059(3) 0.0399(22) Uij ? . C
C9 0.56079(15) 0.3084(5) 0.05078(21) 0.0333(18) Uij ? . C
C10 0.60722(13) 0.2921(5) 0.01661(19) 0.0243(15) Uij ? . C
I 0.00000 0.80200(6) 0.25000 0.04299(21) Uij ? S I
HO1 0.9269(16) 0.073(6) 0.2540(24) 0.0535 Uiso ? . H
HO2 0.820 0.729 0.075 0.0877 Uiso ? . H
HO3 0.7495(22) 0.302(7) 0.261(3) 0.0475 Uiso ? . H
HO4 0.7295(18) 0.797(6) 0.093(3) 0.0444 Uiso ? . H
H1A 0.858 -0.021 0.163 0.0406 Uiso ? . H
H1B 0.813 0.112 0.210 0.0406 Uiso ? . H
H2A 0.893 0.512 0.212 0.0419 Uiso ? . H
H2B 0.817 0.550 0.187 0.0419 Uiso ? . H
H3A 0.694 0.118 0.175 0.0416 Uiso ? . H
H3B 0.653 0.308 0.197 0.0416 Uiso ? . H
H4A 0.640 0.650 0.114 0.0407 Uiso ? . H
H4B 0.655 0.680 0.019 0.0407 Uiso ? . H
H6 0.967 0.368 0.171 0.0418 Uiso ? . H
H7 1.048 0.341 0.108 0.0486 Uiso ? . H
H8 0.469 0.270 0.033 0.0507 Uiso ? . H
H9 0.568 0.360 0.113 0.0437 Uiso ? . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0.002 0.002 'International Tables Vol. IV Table 2.2B'
H ? 0.000 0.000 'International Tables Vol. IV Table 2.2B'
O ? 0.008 0.006 'International Tables Vol. IV Table 2.2B'
P ? 0.090 0.095 'International Tables Vol. IV Table 2.2B'
Re ? -1.598 7.232 'International Tables Vol. IV Table 2.2B'
I ? -0.726 1.812 'International Tables Vol. IV Table 2.2B'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
1 3 5
-5 3 5
-7 3 5
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 Re P1a 179.9 ? ? ? ?
P1 Re P2 99.77(3) ? ? ? ?
P1 Re P2a 80.23(3) ? ? ? ?
P1 Re O5 90.14(7) ? ? ? ?
P1 Re O5a 89.86(7) ? ? ? ?
P1a Re P2 80.23(3) ? ? ? ?
P1a Re P2a 99.77(3) ? ? ? ?
P1a Re O5 89.86(7) ? ? ? ?
P1a Re O5a 90.14(7) ? ? ? ?
P2 Re P2a 180.0 ? ? ? ?
P2 Re O5 88.43(7) ? ? ? ?
P2 Re O5a 91.57(7) ? ? ? ?
P2a Re O5 91.57(7) ? ? ? ?
P2a Re O5a 88.43(7) ? ? ? ?
O5 Re O5a 179.9 ? ? ? ?
Re P1 C1 112.05(11) ? ? ? ?
Re P1 C2 118.51(11) ? ? ? ?
Re P1 C5 109.69(12) ? ? ? ?
C1 P1 C2 104.50(15) ? ? ? ?
C1 P1 C5 106.79(15) ? ? ? ?
C2 P1 C5 104.45(15) ? ? ? ?
Re P2 C3 116.03(13) ? ? ? ?
Re P2 C4 118.28(11) ? ? ? ?
Re P2 C10 109.55(11) ? ? ? ?
C3 P2 C4 105.95(15) ? ? ? ?
C3 P2 C10 104.12(16) ? ? ? ?
C4 P2 C10 101.01(15) ? ? ? ?
C1 O1 Ho1 106(3) ? ? ? ?
C2 O2 Ho2 113.5(3) ? ? ? ?
C3 O3 Ho3 108(4) ? ? ? ?
C4 O4 Ho4 110(3) ? ? ? ?
P1 C1 O1 112.76(23) ? ? ? ?
P1 C1 H1a 108.66(22) ? ? ? ?
P1 C1 H1b 108.42(21) ? ? ? ?
O1 C1 H1a 109.4(3) ? ? ? ?
O1 C1 H1b 108.1(3) ? ? ? ?
H1a C1 H1b 109.5(3) ? ? ? ?
P1 C2 O2 111.52(23) ? ? ? ?
P1 C2 H2a 108.67(23) ? ? ? ?
P1 C2 H2b 108.70(22) ? ? ? ?
O2 C2 H2a 107.7(3) ? ? ? ?
O2 C2 H2b 110.7(3) ? ? ? ?
H2a C2 H2b 109.5(3) ? ? ? ?
P2 C3 O3 107.09(23) ? ? ? ?
P2 C3 H3a 109.8(3) ? ? ? ?
P2 C3 H3b 110.3(3) ? ? ? ?
O3 C3 H3a 109.8(3) ? ? ? ?
O3 C3 H3b 110.3(3) ? ? ? ?
H3a C3 H3b 109.5(3) ? ? ? ?
P2 C4 O4 111.94(22) ? ? ? ?
P2 C4 H4a 109.18(22) ? ? ? ?
P2 C4 H4b 108.66(22) ? ? ? ?
O4 C4 H4a 108.9(3) ? ? ? ?
O4 C4 H4b 108.6(3) ? ? ? ?
H4a C4 H4b 109.5(3) ? ? ? ?
P1 C5 C6 121.5(3) ? ? ? ?
P1 C5 C10a 119.0(3) ? ? ? ?
C6 C5 C10a 119.5(3) ? ? ? ?
C5 C6 C7 119.8(3) ? ? ? ?
C5 C6 H6 119.7(3) ? ? ? ?
C7 C6 H6 120.4(3) ? ? ? ?
C6 C7 C8a 120.7(3) ? ? ? ?
C6 C7 H7 119.6(4) ? ? ? ?
C8a C7 H7 119.7(4) ? ? ? ?
C7a C8 C9 120.1(4) ? ? ? ?
C7a C8 H8 120.0(4) ? ? ? ?
C9 C8 H8 119.9(5) ? ? ? ?
C8 C9 C10 120.3(4) ? ? ? ?
C8 C9 H9 120.0(3) ? ? ? ?
C10 C9 H9 119.7(3) ? ? ? ?
P2 C10 C5a 118.70(24) ? ? ? ?
P2 C10 C9 121.6(3) ? ? ? ?
C5a C10 C9 119.6(3) ? ? ? ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re P1 2.4608(9) ? ? ?
Re P1a 2.4608(9) ? ? ?
Re P2 2.4564(8) ? ? ?
Re P2a 2.4564(8) ? ? ?
Re O5 1.7792(20) ? ? ?
Re O5a 1.7792(20) ? ? ?
P1 C1 1.844(3) ? ? ?
P1 C2 1.837(3) ? ? ?
P1 C5 1.819(4) ? ? ?
P2 C3 1.834(4) ? ? ?
P2 C4 1.844(3) ? ? ?
P2 C10 1.822(3) ? ? ?
O1 C1 1.415(4) ? ? ?
O1 Ho1 0.87(4) ? ? ?
O2 C2 1.389(5) ? ? ?
O2 Ho2 1.080(4) ? ? ?
O3 C3 1.408(5) ? ? ?
O3 Ho3 0.67(5) ? ? ?
O4 C4 1.418(4) ? ? ?
O4 Ho4 0.76(4) ? ? ?
C1 H1a 1.080(3) ? ? ?
C1 H1b 1.080(3) ? ? ?
C2 H2a 1.080(3) ? ? ?
C2 H2b 1.080(3) ? ? ?
C3 H3a 1.080(3) ? ? ?
C3 H3b 1.080(4) ? ? ?
C4 H4a 1.080(3) ? ? ?
C4 H4b 1.080(3) ? ? ?
C5 C6 1.393(5) ? ? ?
C5 C10a 1.409(5) ? ? ?
C6 C7 1.390(5) ? ? ?
C6 H6 1.080(3) ? ? ?
C7 C8a 1.379(7) ? ? ?
C7 H7 1.080(4) ? ? ?
C8 C7a 1.379(7) ? ? ?
C8 C9 1.385(6) ? ? ?
C8 H8 1.080(5) ? ? ?
C9 C10 1.392(5) ? ? ?
C9 H9 1.080(3) ? ? ?
C10 C5a 1.409(5) ? ? ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?
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
? ? ? ? ? ? ? ? ? ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168337561
