#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:15:55 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179319 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/16/4321600.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_4321600
loop_
_publ_author_name
'Daniel Neuman'
'Patrina Paraskevopoulou'
'Nikos Psaroudakis'
'Konstantinos Mertis'
'Richard J. Staples'
'Pericles Stavropoulos'
_publ_section_title
;
 Structural and Functional Characteristics of Rhenium Clusters Derived
 from Redox Chemistry of the Triangular [ReIII3(μ-Cl)3] Core Unit
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5530
_journal_page_last               5537
_journal_paper_doi               10.1021/ic000449t
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety
;
[(C~6~H~5~)~4~P][ReO~4~] 
;
_chemical_formula_sum            'C24 H20 O4 P Re'
_chemical_formula_weight         589.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.262(3)
_cell_length_b                   17.262(3)
_cell_length_c                   14.229(3)
_cell_measurement_reflns_used    108
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.71
_cell_measurement_theta_min      0.00
_cell_volume                     4239.9(14)
_computing_cell_refinement       'SMART (Bruker, V4.050, 1995)'
_computing_data_collection       'ASTRO (Bruker, V4.050, 1995)'
_computing_data_reduction        'SAINT (Bruker, V5.A06, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998, ver 5.10)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.868
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_method       'ω, 0.3 deg'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10107
_diffrn_reflns_theta_full        27.79
_diffrn_reflns_theta_max         27.79
_diffrn_reflns_theta_min         2.36
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.836
_exptl_absorpt_correction_T_max  0.9423
_exptl_absorpt_correction_T_min  0.5000
_exptl_absorpt_correction_type   'empirical, (sadabs)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.147
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.044(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         4266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0048P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0604
_refine_ls_wR_factor_ref         0.0641
_reflns_number_gt                2242
_reflns_number_total             4266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000449t_8.cif
_cod_data_source_block           Compound_9
_cod_original_cell_volume        4240.(1)
_cod_original_sg_symbol_H-M      'P -4'
_cod_database_code               4321600
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re -0.5000 0.0000 -0.2500 0.04055(19) Uani 1 4 d S . .
Re2 Re -0.5000 0.0000 0.2500 0.0460(2) Uani 1 4 d S . .
Re3 Re -0.5000 -0.5000 0.0000 0.03683(16) Uani 1 4 d S . .
Re4 Re 0.0000 0.0000 0.0000 0.0487(2) Uani 1 4 d S . .
O1 O -0.5691(14) -0.0624(15) -0.2709(15) 0.263(14) Uani 0.50 1 d P A 1
O1B O -0.5000 0.0000 -0.3616(11) 0.285(11) Uani 1 2 d S A 2
O2 O -0.5044(4) -0.0750(5) 0.1775(7) 0.179(5) Uani 1 1 d . . .
O3 O -0.5660(4) -0.5417(4) -0.0701(6) 0.146(4) Uani 1 1 d . . .
O4 O 0.0758(8) 0.0008(5) 0.0597(10) 0.328(10) Uani 1 1 d . . .
P1 P -0.75115(16) -0.24068(8) 0.12873(17) 0.0269(3) Uani 1 1 d . . .
C10 C -0.8349(2) -0.2231(2) 0.2006(3) 0.0300(15) Uani 1 1 d G . .
C11 C -0.8798(2) -0.1566(2) 0.1915(3) 0.0353(17) Uani 1 1 d G . .
H11A H -0.8680 -0.1203 0.1455 0.042 Uiso 1 1 calc R . .
C12 C -0.9423(2) -0.1445(2) 0.2514(4) 0.0442(18) Uani 1 1 d G . .
H12A H -0.9723 -0.1001 0.2453 0.053 Uiso 1 1 calc R . .
C13 C -0.95987(19) -0.1989(3) 0.3203(4) 0.053(2) Uani 1 1 d G . .
H13A H -1.0017 -0.1908 0.3603 0.064 Uiso 1 1 calc R . .
C14 C -0.9150(2) -0.2653(2) 0.3293(3) 0.054(2) Uani 1 1 d G . .
H14A H -0.9267 -0.3016 0.3754 0.065 Uiso 1 1 calc R . .
C15 C -0.8525(2) -0.2774(2) 0.2695(3) 0.0400(19) Uani 1 1 d G . .
H15A H -0.8224 -0.3218 0.2755 0.048 Uiso 1 1 calc R . .
C20 C -0.7637(3) -0.3261(2) 0.0588(3) 0.0300(15) Uani 1 1 d G . .
C21 C -0.8284(3) -0.3735(2) 0.0671(3) 0.0348(16) Uani 1 1 d G . .
H21A H -0.8666 -0.3619 0.1110 0.042 Uiso 1 1 calc R . .
C22 C -0.8361(3) -0.4382(2) 0.0097(3) 0.0448(19) Uani 1 1 d G . .
H22A H -0.8794 -0.4700 0.0153 0.054 Uiso 1 1 calc R . .
C23 C -0.7790(3) -0.4555(2) -0.0559(3) 0.0460(19) Uani 1 1 d G . .
H23A H -0.7842 -0.4989 -0.0943 0.055 Uiso 1 1 calc R . .
C24 C -0.7143(3) -0.4081(3) -0.0642(3) 0.0391(17) Uani 1 1 d G . .
H24A H -0.6762 -0.4197 -0.1081 0.047 Uiso 1 1 calc R . .
C25 C -0.7067(2) -0.3434(2) -0.0069(3) 0.0400(16) Uani 1 1 d G . .
H25A H -0.6634 -0.3117 -0.0124 0.048 Uiso 1 1 calc R . .
C30 C -0.7339(3) -0.1613(2) 0.0497(3) 0.0325(16) Uani 1 1 d G . .
C31 C -0.6661(3) -0.1179(3) 0.0532(3) 0.0392(18) Uani 1 1 d G . .
H31A H -0.6291 -0.1281 0.0991 0.047 Uiso 1 1 calc R . .
C32 C -0.6537(3) -0.0591(2) -0.0119(4) 0.047(2) Uani 1 1 d G . .
H32A H -0.6084 -0.0300 -0.0095 0.057 Uiso 1 1 calc R . .
C33 C -0.7090(4) -0.0438(2) -0.0804(3) 0.051(2) Uani 1 1 d G . .
H33A H -0.7007 -0.0045 -0.1240 0.061 Uiso 1 1 calc R . .
C34 C -0.7767(3) -0.0873(3) -0.0839(3) 0.052(2) Uani 1 1 d G . .
H34A H -0.8137 -0.0771 -0.1298 0.062 Uiso 1 1 calc R . .
C35 C -0.7891(3) -0.1461(3) -0.0188(3) 0.048(2) Uani 1 1 d G . .
H35A H -0.8344 -0.1752 -0.0212 0.058 Uiso 1 1 calc R . .
C40 C -0.6699(2) -0.2533(2) 0.2057(3) 0.0287(15) Uani 1 1 d G . .
C41 C -0.6227(2) -0.3185(2) 0.2018(3) 0.0344(16) Uani 1 1 d G . .
H41A H -0.6321 -0.3567 0.1572 0.041 Uiso 1 1 calc R . .
C42 C -0.5615(2) -0.3265(2) 0.2645(4) 0.041(2) Uani 1 1 d G . .
H42A H -0.5300 -0.3701 0.2619 0.049 Uiso 1 1 calc R . .
C43 C -0.54752(19) -0.2693(3) 0.3312(3) 0.0419(17) Uani 1 1 d G . .
H43A H -0.5066 -0.2747 0.3732 0.050 Uiso 1 1 calc R . .
C44 C -0.5947(2) -0.2041(2) 0.3351(3) 0.0465(19) Uani 1 1 d G . .
H44A H -0.5853 -0.1659 0.3797 0.056 Uiso 1 1 calc R . .
C45 C -0.6559(2) -0.1961(2) 0.2723(3) 0.0425(19) Uani 1 1 d G . .
H45A H -0.6874 -0.1525 0.2750 0.051 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'
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'
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 Re1 O1 91.9(3) 7_444 2_455 ?
O1 Re1 O1 91.9(3) 7_444 . ?
O1 Re1 O1 159.1(16) 2_455 . ?
O1 Re1 O1 159.1(16) 7_444 8_454 ?
O1 Re1 O1 91.9(3) 2_455 8_454 ?
O1 Re1 O1 91.9(3) . 8_454 ?
O1 Re1 O1B 100.5(8) 7_444 . ?
O1 Re1 O1B 79.5(8) 2_455 . ?
O1 Re1 O1B 79.5(8) . . ?
O1 Re1 O1B 100.5(8) 8_454 . ?
O1 Re1 O1B 79.5(8) 7_444 7_444 ?
O1 Re1 O1B 100.5(8) 2_455 7_444 ?
O1 Re1 O1B 100.5(8) . 7_444 ?
O1 Re1 O1B 79.5(8) 8_454 7_444 ?
O1B Re1 O1B 180.0 . 7_444 ?
O2 Re2 O2 112.8(4) 8_455 . ?
O2 Re2 O2 103.0(8) 8_455 7_445 ?
O2 Re2 O2 112.8(4) . 7_445 ?
O2 Re2 O2 112.8(4) 8_455 2_455 ?
O2 Re2 O2 103.0(8) . 2_455 ?
O2 Re2 O2 112.8(4) 7_445 2_455 ?
O3 Re3 O3 107.0(7) 2_445 . ?
O3 Re3 O3 110.7(4) 2_445 3_545 ?
O3 Re3 O3 110.7(4) . 3_545 ?
O3 Re3 O3 110.7(4) 2_445 4_455 ?
O3 Re3 O3 110.7(4) . 4_455 ?
O3 Re3 O3 107.0(7) 3_545 4_455 ?
O4 Re4 O4 107.3(6) 4 . ?
O4 Re4 O4 114.0(13) 4 3 ?
O4 Re4 O4 107.3(6) . 3 ?
O4 Re4 O4 107.3(6) 4 2 ?
O4 Re4 O4 114.0(13) . 2 ?
O4 Re4 O4 107.3(6) 3 2 ?
C40 P1 C30 110.2(2) . . ?
C40 P1 C20 109.5(2) . . ?
C30 P1 C20 107.5(3) . . ?
C40 P1 C10 107.6(3) . . ?
C30 P1 C10 111.1(2) . . ?
C20 P1 C10 111.0(2) . . ?
C11 C10 C15 120.0 . . ?
C11 C10 P1 122.4(3) . . ?
C15 C10 P1 117.6(3) . . ?
C10 C11 C12 120.0 . . ?
C11 C12 C13 120.0 . . ?
C14 C13 C12 120.0 . . ?
C15 C14 C13 120.0 . . ?
C14 C15 C10 120.0 . . ?
C21 C20 C25 120.0 . . ?
C21 C20 P1 122.3(3) . . ?
C25 C20 P1 117.7(3) . . ?
C22 C21 C20 120.0 . . ?
C21 C22 C23 120.0 . . ?
C24 C23 C22 120.0 . . ?
C23 C24 C25 120.0 . . ?
C24 C25 C20 120.0 . . ?
C31 C30 C35 120.0 . . ?
C31 C30 P1 121.9(3) . . ?
C35 C30 P1 118.0(3) . . ?
C30 C31 C32 120.0 . . ?
C33 C32 C31 120.0 . . ?
C32 C33 C34 120.0 . . ?
C35 C34 C33 120.0 . . ?
C34 C35 C30 120.0 . . ?
C41 C40 C45 120.0 . . ?
C41 C40 P1 122.1(3) . . ?
C45 C40 P1 117.8(3) . . ?
C40 C41 C42 120.0 . . ?
C43 C42 C41 120.0 . . ?
C42 C43 C44 120.0 . . ?
C43 C44 C45 120.0 . . ?
C44 C45 C40 120.0 . . ?
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
Re1 O1 1.635(10) 7_444 ?
Re1 O1 1.635(10) 2_455 ?
Re1 O1 1.635(10) . ?
Re1 O1 1.635(10) 8_454 ?
Re1 O1B 1.587(15) . ?
Re1 O1B 1.587(15) 7_444 ?
Re2 O2 1.658(7) 8_455 ?
Re2 O2 1.658(7) . ?
Re2 O2 1.658(7) 7_445 ?
Re2 O2 1.658(7) 2_455 ?
Re3 O3 1.677(6) 2_445 ?
Re3 O3 1.677(6) . ?
Re3 O3 1.677(6) 3_545 ?
Re3 O3 1.677(6) 4_455 ?
Re4 O4 1.560(8) 4 ?
Re4 O4 1.560(8) . ?
Re4 O4 1.560(8) 3 ?
Re4 O4 1.560(8) 2 ?
P1 C40 1.793(4) . ?
P1 C30 1.797(4) . ?
P1 C20 1.792(3) . ?
P1 C10 1.797(3) . ?
C10 C11 1.3900 . ?
C10 C15 1.3900 . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C13 C14 1.3900 . ?
C14 C15 1.3900 . ?
C20 C21 1.3900 . ?
C20 C25 1.3900 . ?
C21 C22 1.3900 . ?
C22 C23 1.3900 . ?
C23 C24 1.3900 . ?
C24 C25 1.3900 . ?
C30 C31 1.3900 . ?
C30 C35 1.3900 . ?
C31 C32 1.3900 . ?
C32 C33 1.3900 . ?
C33 C34 1.3900 . ?
C34 C35 1.3900 . ?
C40 C41 1.3900 . ?
C40 C45 1.3900 . ?
C41 C42 1.3900 . ?
C42 C43 1.3900 . ?
C43 C44 1.3900 . ?
C44 C45 1.3900 . ?
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
C40 P1 C10 C11 122.4(3) . . . . ?
C30 P1 C10 C11 1.7(3) . . . . ?
C20 P1 C10 C11 -117.8(3) . . . . ?
C40 P1 C10 C15 -55.2(2) . . . . ?
C30 P1 C10 C15 -175.9(2) . . . . ?
C20 P1 C10 C15 64.6(3) . . . . ?
C15 C10 C11 C12 0.0 . . . . ?
P1 C10 C11 C12 -177.6(3) . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C13 C14 C15 C10 0.0 . . . . ?
C11 C10 C15 C14 0.0 . . . . ?
P1 C10 C15 C14 177.7(3) . . . . ?
C40 P1 C20 C21 114.2(3) . . . . ?
C30 P1 C20 C21 -126.1(3) . . . . ?
C10 P1 C20 C21 -4.4(3) . . . . ?
C40 P1 C20 C25 -67.1(3) . . . . ?
C30 P1 C20 C25 52.6(3) . . . . ?
C10 P1 C20 C25 174.3(2) . . . . ?
C25 C20 C21 C22 0.0 . . . . ?
P1 C20 C21 C22 178.7(3) . . . . ?
C20 C21 C22 C23 0.0 . . . . ?
C21 C22 C23 C24 0.0 . . . . ?
C22 C23 C24 C25 0.0 . . . . ?
C23 C24 C25 C20 0.0 . . . . ?
C21 C20 C25 C24 0.0 . . . . ?
P1 C20 C25 C24 -178.7(3) . . . . ?
C40 P1 C30 C31 -1.0(3) . . . . ?
C20 P1 C30 C31 -120.2(3) . . . . ?
C10 P1 C30 C31 118.2(3) . . . . ?
C40 P1 C30 C35 176.3(3) . . . . ?
C20 P1 C30 C35 57.1(3) . . . . ?
C10 P1 C30 C35 -64.5(3) . . . . ?
C35 C30 C31 C32 0.0 . . . . ?
P1 C30 C31 C32 177.2(4) . . . . ?
C30 C31 C32 C33 0.0 . . . . ?
C31 C32 C33 C34 0.0 . . . . ?
C32 C33 C34 C35 0.0 . . . . ?
C33 C34 C35 C30 0.0 . . . . ?
C31 C30 C35 C34 0.0 . . . . ?
P1 C30 C35 C34 -177.3(3) . . . . ?
C30 P1 C40 C41 -113.1(3) . . . . ?
C20 P1 C40 C41 4.9(3) . . . . ?
C10 P1 C40 C41 125.6(3) . . . . ?
C30 P1 C40 C45 68.5(3) . . . . ?
C20 P1 C40 C45 -173.5(2) . . . . ?
C10 P1 C40 C45 -52.8(3) . . . . ?
C45 C40 C41 C42 0.0 . . . . ?
P1 C40 C41 C42 -178.4(3) . . . . ?
C40 C41 C42 C43 0.0 . . . . ?
C41 C42 C43 C44 0.0 . . . . ?
C42 C43 C44 C45 0.0 . . . . ?
C43 C44 C45 C40 0.0 . . . . ?
C41 C40 C45 C44 0.0 . . . . ?
P1 C40 C45 C44 178.5(3) . . . . ?
