#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:55:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179312 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/09/4320950.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_4320950
loop_
_publ_author_name
'Berthold Nock'
'Theodosia Maina'
'Francesco Tisato'
'Minas Papadopoulos'
'Catherine P. Raptopoulou'
'Aris Terzis'
'Efstratios Chiotellis'
_publ_section_title
;
 Synthesis and Characterization of Six-Coordinate "3 + 2" Mixed-Ligand
 Oxorhenium Complexes with theo-Diphenylphosphinophenolato Ligand and
 Tridentate Coligands of Different N and S Donor Atom Combinations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2178
_journal_page_last               2184
_journal_paper_doi               10.1021/ic991341k
_journal_volume                  39
_journal_year                    2000
_chemical_formula_analytical
ReO{[C2H5SCH2CH2NCH2CH2S][o-C6H4P(C6H5)2]}.0.25CH3OH
_chemical_formula_sum            'C24.25 H28 N O2.25 P Re S2'
_chemical_formula_weight         650.80
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           79
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.00(1)
_cell_length_b                   24.00(1)
_cell_length_c                   8.693(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.7
_cell_measurement_theta_min      5.4
_cell_volume                     5007(4)
_computing_cell_refinement
'Program LEAST (UCLA Crystallographic package, C.E.Strouse, 1994)'
_computing_data_collection
'Program COLLECT (UCLA Crystallographic package, C.E.Strouse, 1994)'
_computing_data_reduction
'Program REDUCE (UCLA Crystallographic package, C.E.Strouse, 1994)'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device
'Crystal Logic Dual Goniometer diffractometer'
_diffrn_measurement_method       'theta-2theta scans'
_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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3722
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        -2.9
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.105
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   'psi-scan empirical'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_meas      1.70
_exptl_crystal_density_method    'floating method'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2564
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.076
_refine_ls_goodness_of_fit_obs   1.077
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         3540
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.076
_refine_ls_restrained_S_obs      1.077
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_obs          0.0378
_refine_ls_shift/esd_max         0.023
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0307P)²+54.6138P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0993
_refine_ls_wR_factor_obs         0.0899
_reflns_number_observed          2944
_reflns_number_total             3540
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic991341k_4.cif
_cod_data_source_block           shel93
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+54.6138P] 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^)+(0.0307P)^2^+54.6138P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5009(1)
_cod_database_code               4320950
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Re Re 0.812223(14) 0.541326(14) 0.78906(11) 0.02762(14) Uani 1 d . .
O1 O 0.8506(5) 0.5287(5) 0.6292(13) 0.042(3) Uani 1 d . .
S1 S 0.82380(14) 0.63607(12) 0.8304(3) 0.0423(9) Uani 1 d . .
N1 N 0.8600(5) 0.5331(6) 0.9727(13) 0.031(3) Uani 1 d . .
S2 S 0.80219(13) 0.43849(12) 0.8171(4) 0.0381(8) Uani 1 d . .
P P 0.7288(2) 0.55886(13) 0.6343(4) 0.0246(7) Uani 1 d . .
O2 O 0.7478(4) 0.5410(4) 0.9538(9) 0.031(2) Uani 1 d . .
C1 C 0.8837(6) 0.6308(6) 0.9589(17) 0.054(4) Uani 1 d . .
H1A H 0.9176(6) 0.6270(6) 0.8991(17) 0.035(25) Uiso 1 calc R .
H1B H 0.8866(6) 0.6644(6) 1.0206(17) 0.035(25) Uiso 1 calc R .
C2 C 0.8766(6) 0.5810(6) 1.0619(16) 0.046(3) Uani 1 d . .
H2A H 0.9114(6) 0.5732(6) 1.1143(16) 0.032(22) Uiso 1 calc R .
H2B H 0.8485(6) 0.5889(6) 1.1391(16) 0.032(22) Uiso 1 calc R .
C3 C 0.8557(6) 0.4821(6) 1.0657(16) 0.048(4) Uani 1 d . .
H3A H 0.8223(6) 0.4841(6) 1.1284(16) 0.030(22) Uiso 1 calc R .
H3B H 0.8874(6) 0.4800(6) 1.1344(16) 0.030(22) Uiso 1 calc R .
C4 C 0.8535(6) 0.4302(6) 0.9696(18) 0.054(4) Uani 1 d . .
H4A H 0.8436(6) 0.3986(6) 1.0337(18) 0.038(24) Uiso 1 calc R .
H4B H 0.8899(6) 0.4231(6) 0.9251(18) 0.038(24) Uiso 1 calc R .
C5 C 0.7375(6) 0.4196(5) 0.9095(17) 0.048(4) Uani 1 d . .
H5A H 0.7347(6) 0.4391(5) 1.0068(17) 0.068(34) Uiso 1 calc R .
H5B H 0.7067(6) 0.4316(5) 0.8453(17) 0.068(34) Uiso 1 calc R .
C6 C 0.7323(6) 0.3570(6) 0.9387(20) 0.060(4) Uani 1 d . .
H6A H 0.6948(15) 0.3485(9) 0.9696(136) 0.115(42) Uiso 1 calc R .
H6B H 0.7576(37) 0.3463(11) 1.0188(98) 0.115(42) Uiso 1 calc R .
H6C H 0.7411(49) 0.3371(6) 0.8462(43) 0.115(42) Uiso 1 calc R .
C7 C 0.6763(4) 0.5690(4) 0.7797(22) 0.029(2) Uani 1 d . .
C8 C 0.6208(5) 0.5866(5) 0.7533(14) 0.040(4) Uani 1 d . .
H8 H 0.6101(5) 0.5990(5) 0.6563(14) 0.050(20) Uiso 1 calc R .
C9 C 0.5831(6) 0.5854(6) 0.8717(17) 0.047(3) Uani 1 d . .
H9 H 0.5463(6) 0.5963(6) 0.8555(17) 0.050(20) Uiso 1 calc R .
C10 C 0.6001(6) 0.5681(6) 1.0133(16) 0.047(4) Uani 1 d . .
H10 H 0.5739(6) 0.5666(6) 1.0921(16) 0.050(20) Uiso 1 calc R .
C11 C 0.6546(6) 0.5527(5) 1.0457(16) 0.045(3) Uani 1 d . .
H11 H 0.6649(6) 0.5420(5) 1.1445(16) 0.050(20) Uiso 1 calc R .
C12 C 0.6940(5) 0.5536(5) 0.9253(14) 0.027(3) Uani 1 d . .
C13 C 0.7276(5) 0.6188(5) 0.5050(12) 0.028(3) Uani 1 d . .
C14 C 0.7140(5) 0.6719(5) 0.5600(15) 0.035(3) Uani 1 d . .
H14 H 0.7053(5) 0.6768(5) 0.6635(15) 0.068(21) Uiso 1 calc R .
C15 C 0.7134(5) 0.7166(5) 0.4631(16) 0.042(3) Uani 1 d . .
H15 H 0.7029(5) 0.7513(5) 0.5012(16) 0.068(21) Uiso 1 calc R .
C16 C 0.7276(5) 0.7120(5) 0.3132(20) 0.041(4) Uani 1 d . .
H16 H 0.7274(5) 0.7432(5) 0.2496(20) 0.068(21) Uiso 1 calc R .
C17 C 0.7427(6) 0.6597(6) 0.2547(15) 0.049(4) Uani 1 d . .
H17 H 0.7522(6) 0.6558(6) 0.1516(15) 0.068(21) Uiso 1 calc R .
C18 C 0.7432(5) 0.6134(5) 0.3524(14) 0.037(3) Uani 1 d . .
H18 H 0.7541(5) 0.5788(5) 0.3148(14) 0.068(21) Uiso 1 calc R .
C19 C 0.7042(5) 0.5022(5) 0.5108(12) 0.027(3) Uani 1 d . .
C20 C 0.6484(5) 0.4914(5) 0.4848(15) 0.039(3) Uani 1 d . .
H20 H 0.6216(5) 0.5133(5) 0.5330(15) 0.060(19) Uiso 1 calc R .
C21 C 0.6318(6) 0.4489(6) 0.3888(15) 0.051(4) Uani 1 d . .
H21 H 0.5941(6) 0.4426(6) 0.3709(15) 0.060(19) Uiso 1 calc R .
C22 C 0.6714(6) 0.4157(6) 0.3192(16) 0.051(4) Uani 1 d . .
H22 H 0.6604(6) 0.3866(6) 0.2557(16) 0.060(19) Uiso 1 calc R .
C23 C 0.7274(6) 0.4257(5) 0.3435(15) 0.051(4) Uani 1 d . .
H23 H 0.7539(6) 0.4032(5) 0.2962(15) 0.060(19) Uiso 1 calc R .
C24 C 0.7442(6) 0.4692(5) 0.4387(14) 0.042(3) Uani 1 d . .
H24 H 0.7819(6) 0.4762(5) 0.4541(14) 0.060(19) Uiso 1 calc R .
CM C 1.0000 0.5000 0.3809(48) 0.043(9) Uiso 0.50 d SP .
OM O 0.9940(14) 0.4737(14) 0.3063(65) 0.060(10) Uiso 0.25 d P .
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'
S S 0.1246 0.1234 '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 Re N1 109.2(4) . . ?
O1 Re O2 162.8(4) . . ?
N1 Re O2 82.9(4) . . ?
O1 Re S1 103.7(4) . . ?
N1 Re S1 84.5(4) . . ?
O2 Re S1 89.2(3) . . ?
O1 Re P 91.4(4) . . ?
N1 Re P 159.4(4) . . ?
O2 Re P 77.0(2) . . ?
S1 Re P 90.83(11) . . ?
O1 Re S2 87.5(4) . . ?
N1 Re S2 83.0(4) . . ?
O2 Re S2 81.9(3) . . ?
S1 Re S2 165.41(11) . . ?
P Re S2 98.34(11) . . ?
C1 S1 Re 97.0(5) . . ?
C2 N1 C3 112.8(11) . . ?
C2 N1 Re 120.9(10) . . ?
C3 N1 Re 119.1(9) . . ?
C5 S2 C4 103.3(7) . . ?
C5 S2 Re 112.1(5) . . ?
C4 S2 Re 96.5(5) . . ?
C7 P C13 108.3(5) . . ?
C7 P C19 106.6(5) . . ?
C13 P C19 102.7(5) . . ?
C7 P Re 102.1(5) . . ?
C13 P Re 119.1(4) . . ?
C19 P Re 117.2(4) . . ?
C12 O2 Re 125.2(7) . . ?
C2 C1 S1 109.3(9) . . ?
N1 C2 C1 110.2(11) . . ?
N1 C3 C4 112.8(12) . . ?
C3 C4 S2 109.8(9) . . ?
C6 C5 S2 113.0(10) . . ?
C12 C7 C8 121.2(14) . . ?
C12 C7 P 112.9(8) . . ?
C8 C7 P 125.8(13) . . ?
C9 C8 C7 119.6(13) . . ?
C10 C9 C8 119.1(12) . . ?
C9 C10 C11 123.2(13) . . ?
C10 C11 C12 118.5(13) . . ?
O2 C12 C7 121.5(10) . . ?
O2 C12 C11 120.1(12) . . ?
C7 C12 C11 118.4(12) . . ?
C18 C13 C14 118.5(11) . . ?
C18 C13 P 120.7(9) . . ?
C14 C13 P 120.7(9) . . ?
C15 C14 C13 120.5(12) . . ?
C16 C15 C14 121.9(12) . . ?
C15 C16 C17 119.2(12) . . ?
C18 C17 C16 119.6(13) . . ?
C13 C18 C17 120.3(12) . . ?
C20 C19 C24 119.3(11) . . ?
C20 C19 P 123.1(9) . . ?
C24 C19 P 117.6(9) . . ?
C21 C20 C19 121.1(13) . . ?
C20 C21 C22 119.6(13) . . ?
C23 C22 C21 120.2(12) . . ?
C22 C23 C24 120.2(12) . . ?
C19 C24 C23 119.5(12) . . ?
OM CM OM 89.8(67) . 2_765 ?
CM OM OM 45.1(34) . 2_765 ?
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 1.694(11) . ?
Re N1 1.976(11) . ?
Re O2 2.107(9) . ?
Re S1 2.319(3) . ?
Re P 2.449(4) . ?
Re S2 2.492(3) . ?
S1 C1 1.825(13) . ?
N1 C2 1.44(2) . ?
N1 C3 1.47(2) . ?
S2 C5 1.807(13) . ?
S2 C4 1.820(14) . ?
P C7 1.80(2) . ?
P C13 1.827(11) . ?
P C19 1.831(11) . ?
O2 C12 1.349(14) . ?
C1 C2 1.50(2) . ?
C3 C4 1.50(2) . ?
C5 C6 1.53(2) . ?
C7 C12 1.39(2) . ?
C7 C8 1.41(2) . ?
C8 C9 1.37(2) . ?
C9 C10 1.36(2) . ?
C10 C11 1.39(2) . ?
C11 C12 1.41(2) . ?
C13 C18 1.38(2) . ?
C13 C14 1.40(2) . ?
C14 C15 1.36(2) . ?
C15 C16 1.35(2) . ?
C16 C17 1.40(2) . ?
C17 C18 1.40(2) . ?
C19 C20 1.38(2) . ?
C19 C24 1.39(2) . ?
C20 C21 1.38(2) . ?
C21 C22 1.38(2) . ?
C22 C23 1.38(2) . ?
C23 C24 1.39(2) . ?
CM OM 0.92(5) . ?
CM OM 0.92(5) 2_765 ?
OM OM 1.29(7) 2_765 ?
