#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:56:43 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179085 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/47/4304753.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_4304753
loop_
_publ_author_name
'Elena López-Torres'
'Ulrich Abram'
_publ_contact_author
;
      Ulrich Abram
      Free University of Berlin     
      Institute of Chemistry             
      Fabeckstrasse 34-36                     
      D-14195 Berlin         
      Germany                          
;
_publ_contact_author_email       abram@chemie.fu-berlin.de
_publ_contact_author_fax         '0049 (0)30 838 52676'
_publ_contact_author_phone       '0049 (0)30 838 54002'
_publ_section_title
;
Rhenium Complexes with Triazine Derivatives Formed from Semicarbazones and
Thiosemicarbazones
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2890
_journal_page_last               2896
_journal_paper_doi               10.1021/ic702326v
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C35 H40 Cl N4 O P2 Re'
_chemical_formula_sum            'C35 H40 Cl N4 O P2 Re'
_chemical_formula_weight         816.30
_chemical_name_common            '[ReNCl(ON)(PEtPh)2]'
_chemical_name_systematic
;
Chlorobis(diethylphenylphosphine)(5,6-diphenyl-1,2,4-triazine-
3-ketonato)nitridorhenium(V)

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/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                 116.10(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.981(2)
_cell_length_b                   24.315(2)
_cell_length_c                   13.531(1)
_cell_measurement_reflns_used    6302
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.29
_cell_measurement_theta_min      2.37
_cell_volume                     3539.9(9)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    ORTEP
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.1435
_diffrn_reflns_av_sigmaI/netI    0.4151
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38137
_diffrn_reflns_theta_full        29.26
_diffrn_reflns_theta_max         29.26
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        1
_exptl_absorpt_coefficient_mu    3.631
_exptl_absorpt_correction_T_max  .7526
_exptl_absorpt_correction_T_min  .3895
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED32'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          .13
_exptl_crystal_size_mid          .09
_exptl_crystal_size_min          .02
_refine_diff_density_max         2.045
_refine_diff_density_min         -1.945
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.685
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         9427
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.685
_refine_ls_R_factor_all          0.2489
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0796P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.2031
_reflns_number_gt                2787
_reflns_number_total             9427
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702326v-file007_2.cif
_cod_data_source_block           rencl(ON)(et2php)2
_cod_original_cell_volume        3539.9(7)
_cod_database_code               4304753
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Re Re 0.28476(7) 0.17078(3) 0.98037(5) 0.03662(19) Uani 1 1 d . . .
N10 N 0.1417(12) 0.1705(6) 0.8947(10) 0.049(3) Uani 1 1 d . . .
Cl Cl 0.3057(5) 0.1969(2) 1.1589(4) 0.0645(14) Uani 1 1 d . . .
O1 O 0.5059(9) 0.1672(5) 1.0359(8) 0.046(2) Uani 1 1 d . . .
C2 C 0.4813(14) 0.1508(5) 0.9373(12) 0.033(3) Uani 1 1 d . . .
N3 N 0.3557(11) 0.1479(5) 0.8740(9) 0.035(3) Uani 1 1 d . . .
N4 N 0.3105(10) 0.1364(4) 0.7688(9) 0.027(3) Uani 1 1 d . . .
C5 C 0.3891(16) 0.1250(6) 0.7288(13) 0.038(4) Uani 1 1 d . . .
C6 C 0.5196(16) 0.1246(6) 0.7947(14) 0.042(4) Uani 1 1 d . . .
N7 N 0.5655(12) 0.1396(5) 0.9000(11) 0.046(3) Uani 1 1 d . . .
C11 C 0.3295(16) 0.1124(7) 0.6073(14) 0.046(4) Uani 1 1 d . . .
C12 C 0.2407(19) 0.0725(9) 0.5695(17) 0.077(7) Uani 1 1 d . . .
H12 H 0.2193 0.0549 0.6198 0.092 Uiso 1 1 calc R . .
C13 C 0.182(3) 0.0569(12) 0.462(2) 0.115(11) Uani 1 1 d . . .
H13 H 0.1310 0.0260 0.4396 0.138 Uiso 1 1 calc R . .
C14 C 0.203(2) 0.0903(15) 0.388(2) 0.126(13) Uani 1 1 d . . .
H14 H 0.1540 0.0852 0.3127 0.151 Uiso 1 1 calc R . .
C15 C 0.292(2) 0.1298(9) 0.4216(16) 0.068(6) Uani 1 1 d . . .
H15 H 0.3091 0.1486 0.3702 0.082 Uiso 1 1 calc R . .
C16 C 0.3586(19) 0.1426(8) 0.5361(13) 0.058(5) Uani 1 1 d . . .
H16 H 0.4188 0.1700 0.5611 0.070 Uiso 1 1 calc R . .
C21 C 0.6132(14) 0.1075(6) 0.7574(13) 0.041(4) Uani 1 1 d . . .
C22 C 0.5928(16) 0.0627(6) 0.6843(15) 0.049(4) Uani 1 1 d . . .
H22 H 0.5166 0.0446 0.6543 0.059 Uiso 1 1 calc R . .
C23 C 0.687(3) 0.0457(10) 0.658(2) 0.093(9) Uani 1 1 d . . .
H23 H 0.6731 0.0164 0.6093 0.112 Uiso 1 1 calc R . .
C24 C 0.798(2) 0.0711(10) 0.700(2) 0.077(7) Uani 1 1 d . . .
H24 H 0.8596 0.0594 0.6805 0.092 Uiso 1 1 calc R . .
C25 C 0.823(2) 0.1140(11) 0.774(2) 0.088(8) Uani 1 1 d . . .
H25 H 0.8996 0.1315 0.8026 0.106 Uiso 1 1 calc R . .
C26 C 0.728(2) 0.1315(8) 0.8047(17) 0.069(6) Uani 1 1 d . . .
H26 H 0.7446 0.1591 0.8568 0.082 Uiso 1 1 calc R . .
P2 P 0.3214(4) 0.26757(16) 0.9491(3) 0.0402(10) Uani 1 1 d . . .
C41 C 0.3723(17) 0.2765(6) 0.8432(13) 0.044(4) Uani 1 1 d . . .
C42 C 0.4984(18) 0.2738(6) 0.8678(15) 0.050(4) Uani 1 1 d . . .
H42 H 0.5585 0.2710 0.9403 0.060 Uiso 1 1 calc R . .
C43 C 0.532(2) 0.2753(6) 0.7822(19) 0.066(6) Uani 1 1 d . . .
H43 H 0.6159 0.2724 0.7984 0.079 Uiso 1 1 calc R . .
C44 C 0.445(2) 0.2809(7) 0.6726(17) 0.064(6) Uani 1 1 d . . .
H44 H 0.4707 0.2824 0.6168 0.077 Uiso 1 1 calc R . .
C45 C 0.326(2) 0.2842(7) 0.6492(16) 0.064(6) Uani 1 1 d . . .
H45 H 0.2668 0.2893 0.5768 0.077 Uiso 1 1 calc R . .
C46 C 0.2880(19) 0.2799(6) 0.7318(15) 0.057(5) Uani 1 1 d . . .
H46 H 0.2034 0.2794 0.7127 0.068 Uiso 1 1 calc R . .
C47 C 0.1827(18) 0.3087(7) 0.9029(16) 0.060(5) Uani 1 1 d . . .
H47A H 0.2020 0.3456 0.8878 0.072 Uiso 1 1 calc R . .
H47B H 0.1211 0.2936 0.8342 0.072 Uiso 1 1 calc R . .
C48 C 0.127(2) 0.3123(7) 0.9820(17) 0.069(6) Uani 1 1 d . . .
H48A H 0.0542 0.3350 0.9513 0.104 Uiso 1 1 calc R . .
H48B H 0.1866 0.3282 1.0497 0.104 Uiso 1 1 calc R . .
H48C H 0.1053 0.2762 0.9958 0.104 Uiso 1 1 calc R . .
C49 C 0.4379(19) 0.3024(7) 1.0707(14) 0.054(5) Uani 1 1 d . . .
H49A H 0.4101 0.3015 1.1281 0.064 Uiso 1 1 calc R . .
H49B H 0.5148 0.2817 1.0969 0.064 Uiso 1 1 calc R . .
C50 C 0.466(2) 0.3632(7) 1.0535(16) 0.067(6) Uani 1 1 d . . .
H50A H 0.5283 0.3776 1.1213 0.100 Uiso 1 1 calc R . .
H50B H 0.3913 0.3846 1.0305 0.100 Uiso 1 1 calc R . .
H50C H 0.4952 0.3648 0.9980 0.100 Uiso 1 1 calc R . .
P1 P 0.2944(5) 0.07403(19) 1.0413(4) 0.0509(12) Uani 1 1 d . . .
C40 C 0.069(2) 0.0730(11) 1.0541(19) 0.104(9) Uani 1 1 d . . .
H40A H 0.0257 0.0644 1.0975 0.155 Uiso 1 1 calc R . .
H40B H 0.0339 0.0521 0.9872 0.155 Uiso 1 1 calc R . .
H40C H 0.0603 0.1116 1.0368 0.155 Uiso 1 1 calc R . .
C31 C 0.2363(14) 0.0243(7) 0.9333(15) 0.048(4) Uani 1 1 d . . .
C33 C 0.1199(16) -0.0020(7) 0.7458(15) 0.053(4) Uani 1 1 d . . .
H33 H 0.0719 0.0093 0.6736 0.063 Uiso 1 1 calc R . .
C32 C 0.1618(17) 0.0385(6) 0.8261(15) 0.051(5) Uani 1 1 d . . .
H32 H 0.1396 0.0751 0.8074 0.061 Uiso 1 1 calc R . .
C37 C 0.457(2) 0.0472(7) 1.1254(17) 0.069(6) Uani 1 1 d . . .
H37A H 0.4537 0.0083 1.1399 0.083 Uiso 1 1 calc R . .
H37B H 0.5056 0.0518 1.0847 0.083 Uiso 1 1 calc R . .
C34 C 0.1422(19) -0.0552(7) 0.763(2) 0.065(6) Uani 1 1 d . . .
H34 H 0.1131 -0.0809 0.7062 0.078 Uiso 1 1 calc R . .
C36 C 0.2613(16) -0.0332(8) 0.9524(15) 0.068(6) Uani 1 1 d . . .
H36 H 0.3131 -0.0459 1.0227 0.081 Uiso 1 1 calc R . .
C35 C 0.209(2) -0.0694(8) 0.868(2) 0.088(8) Uani 1 1 d . . .
H35 H 0.2215 -0.1067 0.8840 0.106 Uiso 1 1 calc R . .
C38 C 0.515(3) 0.0769(8) 1.228(2) 0.127(12) Uani 1 1 d . . .
H38A H 0.5966 0.0626 1.2712 0.190 Uiso 1 1 calc R . .
H38B H 0.4657 0.0725 1.2680 0.190 Uiso 1 1 calc R . .
H38C H 0.5198 0.1152 1.2135 0.190 Uiso 1 1 calc R . .
C39 C 0.205(2) 0.0589(9) 1.1186(14) 0.078(7) Uani 1 1 d . . .
H39A H 0.2135 0.0201 1.1372 0.093 Uiso 1 1 calc R . .
H39B H 0.2398 0.0797 1.1867 0.093 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'
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'
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'
Cl Cl 0.1484 0.1585 '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 Re N3 97.7(5) . . ?
N10 Re Cl 109.7(5) . . ?
N3 Re Cl 152.6(4) . . ?
N10 Re O1 155.3(5) . . ?
N3 Re O1 58.0(4) . . ?
Cl Re O1 94.7(3) . . ?
N10 Re P2 95.5(5) . . ?
N3 Re P2 88.8(3) . . ?
Cl Re P2 88.41(14) . . ?
O1 Re P2 80.4(3) . . ?
N10 Re P1 96.6(5) . . ?
N3 Re P1 90.2(3) . . ?
Cl Re P1 87.01(16) . . ?
O1 Re P1 88.7(3) . . ?
P2 Re P1 167.87(16) . . ?
C2 O1 Re 88.2(8) . . ?
O1 C2 N7 125.6(14) . . ?
O1 C2 N3 110.5(12) . . ?
N7 C2 N3 123.9(13) . . ?
N4 N3 C2 120.4(12) . . ?
N4 N3 Re 136.2(9) . . ?
C2 N3 Re 103.2(9) . . ?
C5 N4 N3 117.8(12) . . ?
N4 C5 C6 122.5(14) . . ?
N4 C5 C11 114.4(14) . . ?
C6 C5 C11 123.1(14) . . ?
N7 C6 C5 119.4(14) . . ?
N7 C6 C21 115.1(15) . . ?
C5 C6 C21 125.4(15) . . ?
C6 N7 C2 115.7(14) . . ?
C12 C11 C16 121.0(19) . . ?
C12 C11 C5 118.1(16) . . ?
C16 C11 C5 120.8(16) . . ?
C13 C12 C11 123(2) . . ?
C12 C13 C14 116(2) . . ?
C15 C14 C13 122(2) . . ?
C14 C15 C16 120(2) . . ?
C11 C16 C15 117(2) . . ?
C26 C21 C22 118.9(16) . . ?
C26 C21 C6 118.6(17) . . ?
C22 C21 C6 122.0(14) . . ?
C23 C22 C21 120(2) . . ?
C24 C23 C22 121(2) . . ?
C23 C24 C25 120.9(18) . . ?
C24 C25 C26 119(2) . . ?
C21 C26 C25 120(2) . . ?
C47 P2 C41 103.9(8) . . ?
C47 P2 C49 106.1(9) . . ?
C41 P2 C49 105.6(8) . . ?
C47 P2 Re 112.6(6) . . ?
C41 P2 Re 113.6(5) . . ?
C49 P2 Re 114.2(6) . . ?
C42 C41 C46 116.9(16) . . ?
C42 C41 P2 120.9(13) . . ?
C46 C41 P2 121.8(14) . . ?
C43 C42 C41 118.8(18) . . ?
C42 C43 C44 122(2) . . ?
C45 C44 C43 119(2) . . ?
C44 C45 C46 120(2) . . ?
C45 C46 C41 122.6(19) . . ?
C48 C47 P2 114.7(13) . . ?
C50 C49 P2 115.7(14) . . ?
C31 P1 C39 102.5(8) . . ?
C31 P1 C37 100.8(8) . . ?
C39 P1 C37 107.0(9) . . ?
C31 P1 Re 115.2(6) . . ?
C39 P1 Re 115.3(8) . . ?
C37 P1 Re 114.4(6) . . ?
C32 C31 C36 115.1(16) . . ?
C32 C31 P1 122.2(13) . . ?
C36 C31 P1 122.7(14) . . ?
C34 C33 C32 125.6(18) . . ?
C31 C32 C33 119.5(16) . . ?
C38 C37 P1 109.8(18) . . ?
C33 C34 C35 115.0(19) . . ?
C35 C36 C31 119.9(18) . . ?
C34 C35 C36 125(2) . . ?
C40 C39 P1 112.3(12) . . ?
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 N10 1.591(13) . ?
Re N3 2.045(11) . ?
Re Cl 2.402(4) . ?
Re O1 2.416(10) . ?
Re P2 2.465(4) . ?
Re P1 2.479(4) . ?
O1 C2 1.296(16) . ?
C2 N7 1.339(18) . ?
C2 N3 1.367(18) . ?
N3 N4 1.311(15) . ?
N4 C5 1.306(17) . ?
C5 C6 1.42(2) . ?
C5 C11 1.51(2) . ?
C6 N7 1.333(19) . ?
C6 C21 1.48(2) . ?
C11 C12 1.36(2) . ?
C11 C16 1.37(2) . ?
C12 C13 1.36(3) . ?
C13 C14 1.40(4) . ?
C14 C15 1.36(3) . ?
C15 C16 1.43(3) . ?
C21 C26 1.37(3) . ?
C21 C22 1.42(2) . ?
C22 C23 1.39(2) . ?
C23 C24 1.35(3) . ?
C24 C25 1.38(3) . ?
C25 C26 1.44(3) . ?
P2 C47 1.800(19) . ?
P2 C41 1.800(17) . ?
P2 C49 1.830(17) . ?
C41 C42 1.40(2) . ?
C41 C46 1.40(2) . ?
C42 C43 1.39(2) . ?
C43 C44 1.39(3) . ?
C44 C45 1.33(3) . ?
C45 C46 1.38(2) . ?
C47 C48 1.49(2) . ?
C49 C50 1.56(2) . ?
P1 C31 1.785(19) . ?
P1 C39 1.83(2) . ?
P1 C37 1.89(2) . ?
C40 C39 1.52(3) . ?
C31 C32 1.37(2) . ?
C31 C36 1.43(2) . ?
C33 C34 1.32(2) . ?
C33 C32 1.39(2) . ?
C37 C38 1.44(3) . ?
C34 C35 1.33(3) . ?
C36 C35 1.36(3) . ?
