#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/48/7104816.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_7104816
loop_
_publ_author_name
'Braband, Henrik'
'Abram, Ulrich'
_publ_section_title
;
 Stable nitridorhenium(V) complexes with an N-heterocyclic carbene
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   19
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2436
_journal_page_last               2437
_journal_paper_doi               10.1039/b307216a
_journal_year                    2003
_chemical_formula_sum            'C41 H29 N8 Re S'
_chemical_formula_weight         851.98
_chemical_name_systematic
;
Isothiocyanato(1,3,4-triphenyl-1,2,4-triazol-5-ylidene)
(1-C6H4-3,4-diphenyl-1,2,4-triazol-5-ylidene)nitridorhenium(V)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 103.11(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.229(3)
_cell_length_b                   12.320(2)
_cell_length_c                   19.344(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.13
_cell_measurement_theta_min      8.49
_cell_volume                     3535.0(8)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        HELENA
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CAD4 ENRAF NONIUS'
_diffrn_measurement_method       omega-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8692
_diffrn_reflns_theta_full        26.97
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         3.09
_diffrn_standards_decay_%        6
_diffrn_standards_interval_count 3600
_diffrn_standards_interval_time  500
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.539
_exptl_absorpt_correction_T_max  0.642
_exptl_absorpt_correction_T_min  0.169
_exptl_absorpt_correction_type   DIFABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.201
_refine_diff_density_min         -2.774
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.790
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         7645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.790
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1380P)²+11.0596P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1677
_reflns_number_gt                5315
_reflns_number_total             7645
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b307216a.txt
_cod_data_source_block           rencarbene2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7104816
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-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 0.28239(2) 0.03682(2) 0.220596(16) 0.04552(13) Uani 1 1 d . . .
N10 N 0.3882(5) 0.0512(7) 0.2209(5) 0.068(2) Uani 1 1 d . . .
C1 C 0.2628(5) 0.1474(6) 0.2980(4) 0.0449(16) Uani 1 1 d . . .
N1 N 0.3251(4) 0.1938(5) 0.3511(3) 0.0478(14) Uani 1 1 d . . .
C11 C 0.4203(5) 0.1706(7) 0.3682(4) 0.0501(18) Uani 1 1 d . . .
C12 C 0.4799(6) 0.2496(8) 0.3593(5) 0.064(2) Uani 1 1 d . . .
H12 H 0.4592 0.3165 0.3401 0.076 Uiso 1 1 calc R . .
C13 C 0.5697(7) 0.2286(10) 0.3791(6) 0.080(3) Uani 1 1 d . . .
H13 H 0.6106 0.2817 0.3726 0.096 Uiso 1 1 calc R . .
C14 C 0.6009(7) 0.1323(12) 0.4079(6) 0.088(4) Uani 1 1 d . . .
H14 H 0.6626 0.1196 0.4212 0.106 Uiso 1 1 calc R . .
C15 C 0.5418(8) 0.0537(9) 0.4176(6) 0.079(3) Uani 1 1 d . . .
H15 H 0.5635 -0.0126 0.4374 0.095 Uiso 1 1 calc R . .
C16 C 0.4490(7) 0.0721(8) 0.3979(5) 0.062(2) Uani 1 1 d . . .
H16 H 0.4080 0.0194 0.4048 0.074 Uiso 1 1 calc R . .
N2 N 0.1847(4) 0.1940(6) 0.3051(3) 0.0508(15) Uani 1 1 d . . .
C21 C 0.0979(5) 0.1735(7) 0.2645(4) 0.0527(19) Uani 1 1 d . . .
C22 C 0.0326(6) 0.2517(8) 0.2579(6) 0.070(3) Uani 1 1 d . . .
H22 H 0.0455 0.3180 0.2809 0.084 Uiso 1 1 calc R . .
C23 C -0.0525(7) 0.2314(10) 0.2168(6) 0.081(3) Uani 1 1 d . . .
H23 H -0.0973 0.2836 0.2138 0.097 Uiso 1 1 calc R . .
C24 C -0.0719(7) 0.1375(10) 0.1812(6) 0.080(3) Uani 1 1 d . . .
H24 H -0.1289 0.1267 0.1522 0.096 Uiso 1 1 calc R . .
C25 C -0.0080(7) 0.0577(9) 0.1876(6) 0.070(3) Uani 1 1 d . . .
H25 H -0.0214 -0.0076 0.1634 0.084 Uiso 1 1 calc R . .
C26 C 0.0775(6) 0.0754(8) 0.2308(5) 0.0556(19) Uani 1 1 d . . .
H26 H 0.1207 0.0208 0.2368 0.067 Uiso 1 1 calc R . .
N3 N 0.1967(5) 0.2711(6) 0.3582(4) 0.0531(16) Uani 1 1 d . . .
C2 C 0.2825(5) 0.2697(6) 0.3863(4) 0.0500(18) Uani 1 1 d . . .
C31 C 0.3278(5) 0.3388(7) 0.4441(4) 0.0508(18) Uani 1 1 d . . .
C32 C 0.3041(7) 0.4475(8) 0.4445(5) 0.067(2) Uani 1 1 d . . .
H32 H 0.2596 0.4757 0.4078 0.080 Uiso 1 1 calc R . .
C33 C 0.3473(9) 0.5146(9) 0.5001(6) 0.077(3) Uani 1 1 d . . .
H33 H 0.3317 0.5876 0.5001 0.092 Uiso 1 1 calc R . .
C34 C 0.4114(8) 0.4743(10) 0.5537(6) 0.077(3) Uani 1 1 d . . .
H34 H 0.4389 0.5194 0.5909 0.092 Uiso 1 1 calc R . .
C35 C 0.4366(7) 0.3667(9) 0.5540(5) 0.069(3) Uani 1 1 d . . .
H35 H 0.4815 0.3395 0.5907 0.083 Uiso 1 1 calc R . .
C36 C 0.3945(7) 0.3000(8) 0.4994(4) 0.064(2) Uani 1 1 d . . .
H36 H 0.4113 0.2274 0.4998 0.077 Uiso 1 1 calc R . .
C3 C 0.2255(5) 0.1389(6) 0.1358(4) 0.0446(16) Uani 1 1 d . . .
N4 N 0.2215(4) 0.2439(5) 0.1158(3) 0.0474(14) Uani 1 1 d . . .
C41 C 0.2615(6) 0.3332(7) 0.1603(4) 0.056(2) Uani 1 1 d . . .
C42 C 0.3527(8) 0.3420(9) 0.1798(5) 0.074(3) Uani 1 1 d . . .
H42 H 0.3894 0.2901 0.1657 0.089 Uiso 1 1 calc R . .
C43 C 0.3902(12) 0.4295(12) 0.2209(7) 0.103(5) Uani 1 1 d . . .
H43 H 0.4526 0.4367 0.2335 0.123 Uiso 1 1 calc R . .
C44 C 0.3390(18) 0.5033(15) 0.2427(8) 0.133(8) Uani 1 1 d . . .
H44 H 0.3655 0.5619 0.2699 0.160 Uiso 1 1 calc R . .
C45 C 0.2465(15) 0.4928(10) 0.2251(8) 0.117(6) Uani 1 1 d . . .
H45 H 0.2113 0.5441 0.2415 0.140 Uiso 1 1 calc R . .
C46 C 0.2041(9) 0.4065(9) 0.1830(6) 0.084(3) Uani 1 1 d . . .
H46 H 0.1418 0.3987 0.1711 0.101 Uiso 1 1 calc R . .
N5 N 0.1739(5) 0.0892(5) 0.0789(3) 0.0487(15) Uani 1 1 d . . .
C51 C 0.1664(6) -0.0255(7) 0.0773(5) 0.0523(19) Uani 1 1 d . . .
C52 C 0.1177(7) -0.0785(8) 0.0186(5) 0.064(2) Uani 1 1 d . . .
H52 H 0.0846 -0.0410 -0.0204 0.077 Uiso 1 1 calc R . .
C53 C 0.1204(7) -0.1911(9) 0.0204(6) 0.074(3) Uani 1 1 d . . .
H53 H 0.0913 -0.2306 -0.0191 0.089 Uiso 1 1 calc R . .
C54 C 0.1659(7) -0.2446(8) 0.0805(6) 0.071(3) Uani 1 1 d . . .
H54 H 0.1649 -0.3200 0.0821 0.085 Uiso 1 1 calc R . .
C55 C 0.2126(6) -0.1872(7) 0.1380(5) 0.058(2) Uani 1 1 d . . .
H55 H 0.2428 -0.2253 0.1778 0.069 Uiso 1 1 calc R . .
C56 C 0.2168(5) -0.0735(7) 0.1390(4) 0.0487(17) Uani 1 1 d . . .
N6 N 0.1367(5) 0.1568(6) 0.0241(3) 0.0530(16) Uani 1 1 d . . .
C4 C 0.1682(5) 0.2529(7) 0.0472(4) 0.0498(18) Uani 1 1 d . . .
C61 C 0.1483(6) 0.3517(7) 0.0049(4) 0.056(2) Uani 1 1 d . . .
C62 C 0.2131(8) 0.4298(8) 0.0052(5) 0.071(3) Uani 1 1 d . . .
H62 H 0.2701 0.4229 0.0349 0.085 Uiso 1 1 calc R . .
C63 C 0.1924(12) 0.5186(8) -0.0393(7) 0.095(4) Uani 1 1 d . . .
H63 H 0.2358 0.5721 -0.0384 0.114 Uiso 1 1 calc R . .
C64 C 0.1109(13) 0.5295(10) -0.0839(7) 0.100(5) Uani 1 1 d . . .
H64 H 0.0978 0.5905 -0.1127 0.120 Uiso 1 1 calc R . .
C65 C 0.0482(10) 0.4506(12) -0.0864(7) 0.101(4) Uani 1 1 d . . .
H65 H -0.0073 0.4565 -0.1182 0.122 Uiso 1 1 calc R . .
C66 C 0.0661(7) 0.3613(9) -0.0419(6) 0.078(3) Uani 1 1 d . . .
H66 H 0.0225 0.3079 -0.0438 0.094 Uiso 1 1 calc R . .
N20 N 0.2799(5) -0.0889(6) 0.2905(4) 0.0581(17) Uani 1 1 d . . .
C20 C 0.2937(6) -0.1597(8) 0.3306(5) 0.060(2) Uani 1 1 d . . .
S20 S 0.3131(3) -0.2596(3) 0.38510(18) 0.0963(10) Uani 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'
Re Re -1.0185 7.2310 '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'
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
N10 Re1 N20 104.3(4) . . ?
N10 Re1 C1 103.2(4) . . ?
N20 Re1 C1 89.6(3) . . ?
N10 Re1 C3 99.9(4) . . ?
N20 Re1 C3 154.1(3) . . ?
C1 Re1 C3 93.9(3) . . ?
N10 Re1 C56 111.6(4) . . ?
N20 Re1 C56 86.1(3) . . ?
C1 Re1 C56 144.9(3) . . ?
C3 Re1 C56 76.3(3) . . ?
N2 C1 N1 103.0(6) . . ?
N2 C1 Re1 128.2(5) . . ?
N1 C1 Re1 128.8(6) . . ?
C1 N1 C2 109.1(6) . . ?
C1 N1 C11 125.8(7) . . ?
C2 N1 C11 125.0(6) . . ?
C12 C11 C16 121.7(8) . . ?
C12 C11 N1 119.5(8) . . ?
C16 C11 N1 118.6(8) . . ?
C13 C12 C11 119.0(10) . . ?
C14 C13 C12 121.3(11) . . ?
C13 C14 C15 120.0(10) . . ?
C14 C15 C16 120.4(10) . . ?
C11 C16 C15 117.7(10) . . ?
C1 N2 N3 113.3(6) . . ?
C1 N2 C21 127.2(7) . . ?
N3 N2 C21 119.4(7) . . ?
C22 C21 C26 119.6(8) . . ?
C22 C21 N2 119.9(8) . . ?
C26 C21 N2 120.6(8) . . ?
C21 C22 C23 119.6(10) . . ?
C24 C23 C22 121.3(10) . . ?
C23 C24 C25 120.2(10) . . ?
C24 C25 C26 119.3(10) . . ?
C21 C26 C25 120.1(9) . . ?
C2 N3 N2 104.7(6) . . ?
N3 C2 N1 109.8(7) . . ?
N3 C2 C31 125.1(7) . . ?
N1 C2 C31 125.1(7) . . ?
C36 C31 C32 118.4(8) . . ?
C36 C31 C2 122.2(8) . . ?
C32 C31 C2 119.5(8) . . ?
C33 C32 C31 119.9(10) . . ?
C34 C33 C32 120.5(10) . . ?
C33 C34 C35 120.6(10) . . ?
C36 C35 C34 119.4(10) . . ?
C35 C36 C31 121.3(9) . . ?
N5 C3 N4 102.7(6) . . ?
N5 C3 Re1 115.4(5) . . ?
N4 C3 Re1 141.9(6) . . ?
C3 N4 C4 109.3(6) . . ?
C3 N4 C41 125.0(7) . . ?
C4 N4 C41 125.6(7) . . ?
C42 C41 C46 122.3(10) . . ?
C42 C41 N4 119.6(9) . . ?
C46 C41 N4 118.1(9) . . ?
C41 C42 C43 119.0(13) . . ?
C44 C43 C42 121.4(16) . . ?
C43 C44 C45 119.9(14) . . ?
C44 C45 C46 121.6(15) . . ?
C45 C46 C41 115.7(13) . . ?
C3 N5 N6 114.9(6) . . ?
C3 N5 C51 119.9(7) . . ?
N6 N5 C51 125.1(6) . . ?
C52 C51 C56 126.5(8) . . ?
C52 C51 N5 121.2(8) . . ?
C56 C51 N5 112.2(7) . . ?
C51 C52 C53 116.6(9) . . ?
C52 C53 C54 120.4(9) . . ?
C55 C54 C53 120.4(9) . . ?
C54 C55 C56 122.7(9) . . ?
C51 C56 C55 113.4(8) . . ?
C51 C56 Re1 115.7(6) . . ?
C55 C56 Re1 130.9(7) . . ?
C4 N6 N5 103.3(6) . . ?
N6 C4 N4 109.8(7) . . ?
N6 C4 C61 123.1(7) . . ?
N4 C4 C61 127.1(7) . . ?
C62 C61 C66 119.1(9) . . ?
C62 C61 C4 121.5(8) . . ?
C66 C61 C4 119.0(8) . . ?
C61 C62 C63 119.2(11) . . ?
C64 C63 C62 121.6(12) . . ?
C63 C64 C65 119.3(11) . . ?
C64 C65 C66 120.7(12) . . ?
C61 C66 C65 120.0(12) . . ?
C20 N20 Re1 168.6(8) . . ?
N20 C20 S20 178.9(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
Re1 N10 1.620(8) . ?
Re1 N20 2.062(7) . ?
Re1 C1 2.095(8) . ?
Re1 C3 2.091(7) . ?
Re1 C56 2.150(8) . ?
C1 N2 1.356(10) . ?
C1 N1 1.356(10) . ?
N1 C2 1.401(10) . ?
N1 C11 1.440(10) . ?
C11 C12 1.367(12) . ?
C11 C16 1.372(12) . ?
C12 C13 1.360(13) . ?
C13 C14 1.351(17) . ?
C14 C15 1.363(17) . ?
C15 C16 1.398(14) . ?
N2 N3 1.380(9) . ?
N2 C21 1.400(10) . ?
C21 C22 1.369(12) . ?
C21 C26 1.374(12) . ?
C22 C23 1.381(14) . ?
C23 C24 1.344(16) . ?
C24 C25 1.369(15) . ?
C25 C26 1.395(13) . ?
N3 C2 1.297(10) . ?
C2 C31 1.449(11) . ?
C31 C36 1.383(12) . ?
C31 C32 1.388(12) . ?
C32 C33 1.396(15) . ?
C33 C34 1.349(17) . ?
C34 C35 1.379(15) . ?
C35 C36 1.376(12) . ?
C3 N5 1.347(10) . ?
C3 N4 1.348(10) . ?
N4 C4 1.393(10) . ?
N4 C41 1.445(10) . ?
C41 C42 1.358(13) . ?
C41 C46 1.396(14) . ?
C42 C43 1.383(16) . ?
C43 C44 1.33(3) . ?
C44 C45 1.38(3) . ?
C45 C46 1.404(19) . ?
N5 N6 1.365(9) . ?
N5 C51 1.418(11) . ?
C51 C52 1.373(12) . ?
C51 C56 1.396(12) . ?
C52 C53 1.387(14) . ?
C53 C54 1.378(14) . ?
C54 C55 1.372(13) . ?
C55 C56 1.402(12) . ?
N6 C4 1.317(10) . ?
C4 C61 1.459(11) . ?
C61 C62 1.378(13) . ?
C61 C66 1.374(13) . ?
C62 C63 1.384(14) . ?
C63 C64 1.35(2) . ?
C64 C65 1.36(2) . ?
C65 C66 1.384(16) . ?
N20 C20 1.155(11) . ?
C20 S20 1.604(10) . ?
