#------------------------------------------------------------------------------
#$Date: 2019-11-25 01:04:52 +0200 (Mon, 25 Nov 2019) $
#$Revision: 239832 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/03/4350305.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_4350305
loop_
_publ_author_name
'Chiotellis, Aris'
'Tsoukalas, Charalambos'
'Pelecanou, Maria'
'Papadopoulos, Apostolos'
'Raptopoulou, Catherine'
'Terzis, Aris'
'Pirmettis, Ioannis'
'Papadopoulos, Minas'
'Chiotellis, Efstratios'
_publ_section_title
;
 Synthesis and characterization of novel "3 + 2" oxorhenium
 complexes, ReO[SNO][NN].
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5635
_journal_page_last               5640
_journal_paper_doi               10.1021/ic0604260
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C24 H30 N5 O5 Re S'
_chemical_formula_weight         686.79
_space_group_IT_number           15
_space_group_name_Hall           '-A 2yab'
_space_group_name_H-M_alt        'A 1 2/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'A 1 2/n 1'
_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                 91.87(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.269(6)
_cell_length_b                   10.548(5)
_cell_length_c                   33.90(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.7
_cell_measurement_theta_min      5.4
_cell_volume                     5100(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Crystal Logic Dual Goniometer'
_diffrn_measurement_method       θ/2θ
_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  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4567
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        2.9
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.893
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   'psi-scan empirical'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parall
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.993
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         4483
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0351P)²+42.3167P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1022
_reflns_number_gt                3739
_reflns_number_total             4483
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0604260si20060313_102009.cif
_cod_data_source_block           COMPOUND_5
_cod_original_cell_volume        5099(4)
_cod_original_sg_symbol_H-M      A2/n
_cod_database_code               4350305
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'x, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1'
'-x, -y, -z'
'x-1/2, -y, z-1/2'
'-x, -y+1/2, -z+1/2'
'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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Re1 Re 0.401835(17) 0.53499(2) 0.649431(8) 0.03203(11) Uani 1 1 d .
S S 0.27096(12) 0.62054(19) 0.67692(6) 0.0466(4) Uani 1 1 d .
O1 O 0.3979(4) 0.5894(6) 0.60312(15) 0.0497(13) Uani 1 1 d .
O2 O 0.5333(3) 0.4551(5) 0.65382(17) 0.0441(12) Uani 1 1 d .
N1 N 0.4689(4) 0.6620(6) 0.68209(17) 0.0393(13) Uani 1 1 d .
N2 N 0.3909(4) 0.4001(6) 0.70169(17) 0.0360(12) Uani 1 1 d .
N3 N 0.3385(4) 0.3635(5) 0.62901(17) 0.0351(12) Uani 1 1 d .
O3 O 0.6820(4) 0.4905(6) 0.6697(2) 0.0618(16) Uani 1 1 d .
O4 O 0.4736(5) 0.8513(6) 0.71387(18) 0.0645(16) Uani 1 1 d .
O5 O -0.2608(4) 0.3816(5) 0.52566(16) 0.0522(13) Uani 1 1 d .
N4 N 0.0532(4) 0.4681(6) 0.59303(17) 0.0360(13) Uani 1 1 d .
N5 N -0.1460(4) 0.4967(5) 0.57978(16) 0.0317(12) Uani 1 1 d .
C1 C 0.3246(7) 0.7594(9) 0.7005(3) 0.055(2) Uani 1 1 d .
C2 C 0.4296(6) 0.7626(7) 0.6998(2) 0.0458(17) Uani 1 1 d .
C3 C 0.5716(5) 0.6532(8) 0.6831(3) 0.0485(19) Uani 1 1 d .
C4 C 0.6003(5) 0.5257(7) 0.6678(2) 0.0427(17) Uani 1 1 d .
C5 C 0.4133(6) 0.4284(9) 0.7386(2) 0.0486(19) Uani 1 1 d .
C6 C 0.4046(6) 0.3416(11) 0.7688(3) 0.062(2) Uani 1 1 d .
C7 C 0.3733(6) 0.2214(11) 0.7601(3) 0.069(3) Uani 1 1 d .
C8 C 0.3495(6) 0.1905(9) 0.7215(3) 0.061(3) Uani 1 1 d .
C9 C 0.3574(4) 0.2840(7) 0.6930(2) 0.0393(16) Uani 1 1 d .
C10 C 0.3281(5) 0.2694(7) 0.6519(3) 0.0437(18) Uani 1 1 d .
C11 C 0.3065(5) 0.3485(8) 0.5872(2) 0.0476(18) Uani 1 1 d .
H11A H 0.2935 0.2598 0.5819 0.062(18) Uiso 1 1 calc R
H11B H 0.3561 0.3753 0.5702 0.062(18) Uiso 1 1 calc R
C12 C 0.2190(5) 0.4262(8) 0.5780(2) 0.0436(17) Uani 1 1 d .
C13 C 0.1379(5) 0.3969(9) 0.6039(3) 0.0457(17) Uani 1 1 d .
C14 C 0.0049(5) 0.4161(9) 0.5584(2) 0.0439(18) Uani 1 1 d .
C15 C -0.0804(5) 0.4941(9) 0.5472(2) 0.0438(17) Uani 1 1 d .
C16 C -0.0972(5) 0.5486(8) 0.6148(2) 0.0410(16) Uani 1 1 d .
C17 C -0.0119(5) 0.4716(9) 0.6254(2) 0.0418(17) Uani 1 1 d .
C18 C -0.2349(5) 0.5520(6) 0.5697(2) 0.0336(14) Uani 1 1 d .
C19 C -0.2944(5) 0.4909(7) 0.5414(2) 0.0419(16) Uani 1 1 d .
C20 C -0.3799(6) 0.5418(10) 0.5313(3) 0.061(2) Uani 1 1 d .
C21 C -0.4101(6) 0.6539(10) 0.5491(4) 0.073(3) Uani 1 1 d .
C22 C -0.3555(7) 0.7116(9) 0.5772(3) 0.061(2) Uani 1 1 d .
C23 C -0.2673(5) 0.6617(7) 0.5875(2) 0.0433(17) Uani 1 1 d .
C24 C -0.3184(8) 0.3199(10) 0.4976(3) 0.059(2) Uiso 1 1 d .
H1A H 0.304(5) 0.823(8) 0.689(2) 0.04(2) Uiso 1 1 d .
H1B H 0.303(6) 0.761(8) 0.724(3) 0.05(2) Uiso 1 1 d .
H3A H 0.593(6) 0.733(10) 0.668(3) 0.06(3) Uiso 1 1 d .
H3B H 0.594(7) 0.664(10) 0.707(3) 0.07(3) Uiso 1 1 d .
H5 H 0.436(6) 0.506(8) 0.744(2) 0.05(2) Uiso 1 1 d .
H6 H 0.415(5) 0.370(8) 0.794(2) 0.04(2) Uiso 1 1 d .
H7 H 0.366(8) 0.169(12) 0.779(3) 0.10(4) Uiso 1 1 d .
H8 H 0.326(8) 0.125(12) 0.716(3) 0.08(4) Uiso 1 1 d .
H10 H 0.302(8) 0.200(12) 0.643(3) 0.10(4) Uiso 1 1 d .
H12A H 0.234(5) 0.531(6) 0.5809(19) 0.025(16) Uiso 1 1 d .
H12B H 0.208(5) 0.420(8) 0.553(2) 0.04(2) Uiso 1 1 d .
H13A H 0.125(5) 0.316(8) 0.603(2) 0.04(2) Uiso 1 1 d .
H13B H 0.149(7) 0.397(10) 0.632(3) 0.08(3) Uiso 1 1 d .
H14A H -0.012(7) 0.329(11) 0.562(3) 0.07(3) Uiso 1 1 d .
H14B H 0.042(6) 0.423(8) 0.539(2) 0.04(2) Uiso 1 1 d .
H15A H -0.057(6) 0.585(10) 0.541(3) 0.06(3) Uiso 1 1 d .
H15B H -0.110(7) 0.454(9) 0.527(3) 0.07(3) Uiso 1 1 d .
H16A H -0.140(4) 0.562(5) 0.6373(16) 0.007(12) Uiso 1 1 d .
H16B H -0.072(6) 0.627(8) 0.611(2) 0.05(2) Uiso 1 1 d .
H17A H -0.025(5) 0.385(7) 0.635(2) 0.032(18) Uiso 1 1 d .
H17B H 0.015(5) 0.488(7) 0.646(2) 0.030(19) Uiso 1 1 d .
H20 H -0.418(8) 0.498(11) 0.513(3) 0.09(4) Uiso 1 1 d .
H21 H -0.465(6) 0.681(9) 0.542(2) 0.06(2) Uiso 1 1 d .
H22 H -0.367(6) 0.782(9) 0.588(2) 0.05(2) Uiso 1 1 d .
H23 H -0.233(4) 0.702(6) 0.6075(19) 0.020(15) Uiso 1 1 d .
H24A H -0.372(6) 0.302(8) 0.509(2) 0.04(2) Uiso 1 1 d .
H24B H -0.283(5) 0.273(7) 0.4903(19) 0.027(17) Uiso 1 1 d .
H24C H -0.333(7) 0.387(11) 0.473(3) 0.08(3) Uiso 1 1 d .
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'
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
O1 Re1 N1 107.2(3)
O1 Re1 O2 102.2(2)
N1 Re1 O2 79.2(2)
O1 Re1 N3 89.2(3)
N1 Re1 N3 163.0(2)
O2 Re1 N3 93.0(2)
O1 Re1 N2 160.5(3)
N1 Re1 N2 91.8(2)
O2 Re1 N2 76.9(2)
N3 Re1 N2 71.5(2)
O1 Re1 S 104.1(2)
N1 Re1 S 83.73(18)
O2 Re1 S 151.93(17)
N3 Re1 S 97.08(16)
N2 Re1 S 81.54(15)
C1 S Re1 99.1(3)
C4 O2 Re1 116.9(5)
C2 N1 C3 117.9(6)
C2 N1 Re1 125.8(5)
C3 N1 Re1 115.9(5)
C5 N2 C9 119.2(7)
C5 N2 Re1 125.2(6)
C9 N2 Re1 115.6(5)
C10 N3 C11 117.5(6)
C10 N3 Re1 121.4(5)
C11 N3 Re1 121.1(5)
C19 O5 C24 117.0(7)
C14 N4 C13 112.1(6)
C14 N4 C17 108.6(6)
C13 N4 C17 111.4(6)
C18 N5 C16 115.9(6)
C18 N5 C15 114.2(5)
C16 N5 C15 108.7(6)
C2 C1 S 114.6(6)
O4 C2 N1 124.2(8)
O4 C2 C1 121.0(8)
N1 C2 C1 114.8(7)
N1 C3 C4 109.4(6)
O3 C4 O2 122.5(8)
O3 C4 C3 121.6(7)
O2 C4 C3 115.9(6)
N2 C5 C6 121.9(9)
C7 C6 C5 119.4(10)
C6 C7 C8 119.3(9)
C7 C8 C9 117.9(10)
N2 C9 C8 122.2(8)
N2 C9 C10 113.3(6)
C8 C9 C10 124.4(8)
N3 C10 C9 117.9(7)
N3 C11 C12 111.3(6)
C13 C12 C11 114.4(7)
N4 C13 C12 113.2(7)
N4 C14 C15 110.9(7)
N5 C15 C14 110.3(6)
N5 C16 C17 110.7(6)
N4 C17 C16 111.5(6)
C23 C18 C19 118.1(7)
C23 C18 N5 122.8(6)
C19 C18 N5 119.0(6)
O5 C19 C20 123.8(8)
O5 C19 C18 116.1(6)
C20 C19 C18 120.1(8)
C19 C20 C21 120.6(9)
C22 C21 C20 120.2(8)
C21 C22 C23 119.8(9)
C18 C23 C22 121.0(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Re1 O1 1.670(5)
Re1 N1 1.967(6)
Re1 O2 2.058(5)
Re1 N3 2.127(6)
Re1 N2 2.281(6)
Re1 S 2.299(2)
S C1 1.825(10)
O2 C4 1.291(9)
N1 C2 1.350(10)
N1 C3 1.468(10)
N2 C5 1.317(10)
N2 C9 1.343(9)
N3 C10 1.272(10)
N3 C11 1.482(9)
O3 C4 1.223(9)
O4 C2 1.215(9)
O5 C19 1.364(9)
O5 C24 1.399(11)
N4 C14 1.449(10)
N4 C13 1.459(9)
N4 C17 1.461(9)
N5 C18 1.428(8)
N5 C16 1.463(9)
N5 C15 1.472(9)
C1 C2 1.499(12)
C3 C4 1.503(11)
C5 C6 1.380(12)
C6 C7 1.373(15)
C7 C8 1.381(16)
C8 C9 1.386(11)
C9 C10 1.450(11)
C11 C12 1.517(10)
C12 C13 1.505(11)
C14 C15 1.507(10)
C16 C17 1.498(11)
C18 C23 1.390(10)
C18 C19 1.414(10)
C19 C20 1.366(11)
C20 C21 1.401(14)
C21 C22 1.356(15)
C22 C23 1.398(12)
