#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:34:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179452 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/49/4334996.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_4334996
loop_
_publ_author_name
'Hayato Ikeda'
'Akitaka Ito'
'Eri Sakuda'
'Noboru Kitamura'
'Tsutomu Takayama'
'Tsutomu Sekine'
'Atsushi Shinohara'
'Takashi Yoshimura'
_publ_section_title
;
 Excited-State Characteristics of Tetracyanidonitridorhenium(V) and
 -technetium(V) Complexes with N-Heteroaromatic Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6319
_journal_page_last               6327
_journal_paper_doi               10.1021/ic302463v
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C62 H50 N7 O P2 Re'
_chemical_formula_sum            'C62 H50 N7 O P2 Re'
_chemical_formula_weight         1157.28
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   17.3282(6)
_cell_length_b                   23.0629(6)
_cell_length_c                   13.5233(4)
_cell_measurement_reflns_used    38065
_cell_measurement_temperature    170
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.02
_cell_volume                     5404.4(3)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF99-PATTY (Gould, et al., 1999)'
_diffrn_ambient_temperature      170
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0993
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            50576
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.357
_exptl_absorpt_correction_T_max  0.772
_exptl_absorpt_correction_T_min  0.618
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(Walker & Stuart, 1983)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       prism
_exptl_crystal_F_000             2336.00
_exptl_crystal_size_max          0.620
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.130
_refine_diff_density_min         -0.710
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.848
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6350
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0368P)²+11.7068P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0770
_reflns_number_gt                5587
_reflns_number_total             6350
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ic302463v_si_002_05.cif
_cod_data_source_block           (PPh4)2[ReN(CN)4(py)]
_cod_database_code               4334996
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2+Z
3 +X,1/2-Y,+Z
4 1/2-X,-Y,1/2+Z
5 -X,-Y,-Z
6 1/2+X,1/2-Y,1/2-Z
7 -X,1/2+Y,-Z
8 1/2+X,+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 -0.015711(8) 0.7500 0.823052(11) 0.01808(6) Uani 1.0 4 d .
P1 P 0.20811(4) 0.45963(3) 0.67364(6) 0.02210(15) Uani 1.0 8 d .
O1 O 0.0652(2) 0.2500 0.7289(3) 0.0467(9) Uani 1.0 4 d .
N1 N -0.1101(2) 0.7500 0.8036(3) 0.0278(8) Uani 1.0 4 d .
N2 N 0.0475(2) 0.7500 0.5959(3) 0.0310(8) Uani 1.0 4 d .
N3 N 0.00725(17) 0.60959(13) 0.8204(2) 0.0352(7) Uani 1.0 8 d .
N4 N -0.0216(2) 0.7500 1.0636(3) 0.0375(10) Uani 1.0 4 d .
N5 N 0.1290(2) 0.7500 0.8610(3) 0.0240(7) Uani 1.0 4 d .
N7 N 0.2261(2) 0.2500 0.7718(4) 0.0433(11) Uani 1.0 4 d .
C1 C 0.0251(2) 0.7500 0.6765(3) 0.0226(9) Uani 1.0 4 d .
C2 C 0.00021(17) 0.65900(13) 0.8234(2) 0.0235(6) Uani 1.0 8 d .
C3 C -0.0190(2) 0.7500 0.9785(3) 0.0246(9) Uani 1.0 4 d .
C4 C 0.1693(3) 0.70172(16) 0.8714(4) 0.0586(13) Uani 1.0 8 d .
C5 C 0.2469(3) 0.70000(17) 0.8938(5) 0.0664(15) Uani 1.0 8 d .
C6 C 0.2864(3) 0.7500 0.9041(4) 0.0375(11) Uani 1.0 4 d .
C7 C 0.21697(17) 0.53583(12) 0.6505(3) 0.0240(6) Uani 1.0 8 d .
C8 C 0.28676(19) 0.56369(13) 0.6710(3) 0.0306(7) Uani 1.0 8 d .
C9 C 0.2915(3) 0.62363(14) 0.6637(3) 0.0410(9) Uani 1.0 8 d .
C10 C 0.2280(3) 0.65524(14) 0.6349(4) 0.0477(10) Uani 1.0 8 d .
C11 C 0.1589(2) 0.62799(14) 0.6131(4) 0.0446(9) Uani 1.0 8 d .
C12 C 0.15282(18) 0.56836(13) 0.6212(3) 0.0338(8) Uani 1.0 8 d .
C13 C 0.16295(17) 0.44956(12) 0.7912(3) 0.0244(6) Uani 1.0 8 d .
C14 C 0.12195(18) 0.49487(13) 0.8349(3) 0.0285(7) Uani 1.0 8 d .
C15 C 0.08732(19) 0.48645(14) 0.9259(3) 0.0353(8) Uani 1.0 8 d .
C16 C 0.0927(2) 0.43338(15) 0.9733(3) 0.0378(8) Uani 1.0 8 d .
C17 C 0.1330(2) 0.38788(15) 0.9298(3) 0.0373(8) Uani 1.0 8 d .
C18 C 0.1684(2) 0.39576(13) 0.8397(3) 0.0318(7) Uani 1.0 8 d .
C19 C 0.30194(18) 0.42679(12) 0.6786(3) 0.0276(7) Uani 1.0 8 d .
C20 C 0.3351(2) 0.40309(14) 0.5947(3) 0.0383(8) Uani 1.0 8 d .
C21 C 0.4089(3) 0.37995(17) 0.5998(4) 0.0504(11) Uani 1.0 8 d .
C22 C 0.4486(3) 0.37967(18) 0.6867(4) 0.0537(12) Uani 1.0 8 d .
C23 C 0.4168(2) 0.40373(17) 0.7706(4) 0.0493(10) Uani 1.0 8 d .
C24 C 0.34267(19) 0.42705(15) 0.7671(3) 0.0397(8) Uani 1.0 8 d .
C25 C 0.15117(16) 0.42700(12) 0.5777(3) 0.0248(6) Uani 1.0 8 d .
C26 C 0.1479(2) 0.45179(14) 0.4837(3) 0.0340(7) Uani 1.0 8 d .
C27 C 0.1027(3) 0.42631(15) 0.4112(3) 0.0402(8) Uani 1.0 8 d .
C28 C 0.06255(19) 0.37610(15) 0.4298(3) 0.0371(8) Uani 1.0 8 d .
C29 C 0.06673(19) 0.35063(14) 0.5224(3) 0.0356(8) Uani 1.0 8 d .
C30 C 0.11044(18) 0.37594(13) 0.5967(3) 0.0301(7) Uani 1.0 8 d .
C31 C 0.2838(3) 0.2500 0.7051(4) 0.0432(12) Uani 1.0 4 d .
C32 C 0.3604(3) 0.2500 0.7322(5) 0.0483(14) Uani 1.0 4 d .
C33 C 0.3789(3) 0.2500 0.8311(5) 0.0511(15) Uani 1.0 4 d .
C34 C 0.3210(3) 0.2500 0.8988(4) 0.0468(13) Uani 1.0 4 d .
C35 C 0.2462(3) 0.2500 0.8664(4) 0.0432(13) Uani 1.0 4 d .
H4 H 0.1431 0.6659 0.8628 0.0704 Uiso 1.0 8 calc R
H5 H 0.2723 0.6638 0.9020 0.0797 Uiso 1.0 8 calc R
H6 H 0.3401 0.7500 0.9181 0.0449 Uiso 1.0 4 calc R
H8 H 0.3307 0.5417 0.6899 0.0367 Uiso 1.0 8 calc R
H9 H 0.3386 0.6428 0.6786 0.0492 Uiso 1.0 8 calc R
H10 H 0.2317 0.6962 0.6299 0.0573 Uiso 1.0 8 calc R
H11 H 0.1157 0.6502 0.5925 0.0536 Uiso 1.0 8 calc R
H12 H 0.1053 0.5496 0.6069 0.0406 Uiso 1.0 8 calc R
H14 H 0.1179 0.5313 0.8025 0.0342 Uiso 1.0 8 calc R
H15 H 0.0596 0.5173 0.9561 0.0424 Uiso 1.0 8 calc R
H16 H 0.0688 0.4280 1.0358 0.0453 Uiso 1.0 8 calc R
H17 H 0.1361 0.3514 0.9622 0.0447 Uiso 1.0 8 calc R
H18 H 0.1964 0.3649 0.8103 0.0381 Uiso 1.0 8 calc R
H20 H 0.3074 0.4027 0.5340 0.0459 Uiso 1.0 8 calc R
H21 H 0.4320 0.3642 0.5420 0.0605 Uiso 1.0 8 calc R
H22 H 0.4985 0.3628 0.6896 0.0644 Uiso 1.0 8 calc R
H23 H 0.4453 0.4044 0.8306 0.0592 Uiso 1.0 8 calc R
H24 H 0.3201 0.4431 0.8250 0.0477 Uiso 1.0 8 calc R
H26 H 0.1765 0.4859 0.4695 0.0408 Uiso 1.0 8 calc R
H27 H 0.0995 0.4438 0.3478 0.0482 Uiso 1.0 8 calc R
H28 H 0.0320 0.3589 0.3793 0.0445 Uiso 1.0 8 calc R
H29 H 0.0395 0.3156 0.5351 0.0427 Uiso 1.0 8 calc R
H30 H 0.1127 0.3586 0.6604 0.0362 Uiso 1.0 8 calc R
H31 H 0.2712 0.2500 0.6367 0.0518 Uiso 1.0 4 calc R
H32 H 0.3998 0.2500 0.6834 0.0579 Uiso 1.0 4 calc R
H33 H 0.4313 0.2500 0.8517 0.0613 Uiso 1.0 4 calc R
H34 H 0.3323 0.2500 0.9676 0.0562 Uiso 1.0 4 calc R
H35 H 0.2063 0.2500 0.9146 0.0518 Uiso 1.0 4 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 for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
P P 0.1023 0.0942
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Re Re -1.0185 7.2310
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(1992, 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_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Re1 N5 177.57(17) yes . .
N1 Re1 C1 100.50(17) yes . .
N1 Re1 C2 97.41(8) yes . .
N1 Re1 C2 97.41(8) yes . 3_565
N1 Re1 C3 97.58(17) yes . .
N5 Re1 C1 81.93(14) yes . .
N5 Re1 C2 82.64(8) yes . .
N5 Re1 C2 82.64(8) yes . 3_565
N5 Re1 C3 79.99(13) yes . .
C1 Re1 C2 87.62(8) yes . .
C1 Re1 C2 87.62(8) yes . 3_565
C1 Re1 C3 161.92(14) yes . .
C2 Re1 C2 165.02(12) yes . 3_565
C2 Re1 C3 90.07(8) yes . .
C2 Re1 C3 90.07(8) yes 3_565 .
C7 P1 C13 108.69(14) yes . .
C7 P1 C19 110.05(14) yes . .
C7 P1 C25 109.38(14) yes . .
C13 P1 C19 107.96(15) yes . .
C13 P1 C25 110.36(14) yes . .
C19 P1 C25 110.37(14) yes . .
Re1 N5 C4 122.6(2) yes . .
Re1 N5 C4 122.6(2) yes . 3_565
C4 N5 C4 114.8(4) yes . 3_565
C31 N7 C35 116.8(5) yes . .
Re1 C1 N2 180.0(4) yes . .
Re1 C2 N3 177.4(3) yes . .
Re1 C3 N4 179.3(4) yes . .
N5 C4 C5 124.2(4) yes . .
C4 C5 C6 119.6(4) yes . .
C5 C6 C5 117.5(5) yes . 3_565
P1 C7 C8 119.4(3) yes . .
P1 C7 C12 120.5(3) yes . .
C8 C7 C12 119.8(3) yes . .
C7 C8 C9 119.7(3) yes . .
C8 C9 C10 120.1(4) yes . .
C9 C10 C11 120.7(3) yes . .
C10 C11 C12 120.0(4) yes . .
C7 C12 C11 119.7(3) yes . .
P1 C13 C14 120.2(3) yes . .
P1 C13 C18 120.0(3) yes . .
C14 C13 C18 119.8(3) yes . .
C13 C14 C15 119.6(3) yes . .
C14 C15 C16 120.4(3) yes . .
C15 C16 C17 120.3(4) yes . .
C16 C17 C18 119.9(4) yes . .
C13 C18 C17 120.0(3) yes . .
P1 C19 C20 120.7(3) yes . .
P1 C19 C24 119.4(3) yes . .
C20 C19 C24 119.8(3) yes . .
C19 C20 C21 119.6(4) yes . .
C20 C21 C22 120.6(4) yes . .
C21 C22 C23 120.5(4) yes . .
C22 C23 C24 119.7(4) yes . .
C19 C24 C23 119.8(4) yes . .
P1 C25 C26 120.6(3) yes . .
P1 C25 C30 119.8(3) yes . .
C26 C25 C30 119.6(3) yes . .
C25 C26 C27 119.6(3) yes . .
C26 C27 C28 121.0(4) yes . .
C27 C28 C29 119.7(4) yes . .
C28 C29 C30 120.4(3) yes . .
C25 C30 C29 119.8(3) yes . .
N7 C31 C32 122.5(6) yes . .
C31 C32 C33 118.9(6) yes . .
C32 C33 C34 118.9(5) yes . .
C33 C34 C35 118.9(6) yes . .
N7 C35 C34 123.9(5) yes . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_2
Re1 N1 1.657(4) yes .
Re1 N5 2.560(4) yes .
Re1 C1 2.104(4) yes .
Re1 C2 2.117(3) yes .
Re1 C2 2.117(3) yes 3_565
Re1 C3 2.103(4) yes .
P1 C7 1.792(3) yes .
P1 C13 1.787(4) yes .
P1 C19 1.795(4) yes .
P1 C25 1.796(3) yes .
N2 C1 1.157(6) yes .
N3 C2 1.147(5) yes .
N4 C3 1.152(6) yes .
N5 C4 1.322(5) yes .
N5 C4 1.322(5) yes 3_565
N7 C31 1.347(7) yes .
N7 C35 1.326(8) yes .
C4 C5 1.379(6) yes .
C5 C6 1.349(5) yes .
C7 C8 1.397(5) yes .
C7 C12 1.398(5) yes .
C8 C9 1.388(5) yes .
C9 C10 1.376(6) yes .
C10 C11 1.384(6) yes .
C11 C12 1.384(5) yes .
C13 C14 1.395(5) yes .
C13 C18 1.407(5) yes .
C14 C15 1.382(5) yes .
C15 C16 1.385(5) yes .
C16 C17 1.391(5) yes .
C17 C18 1.376(5) yes .
C19 C20 1.384(5) yes .
C19 C24 1.388(5) yes .
C20 C21 1.389(6) yes .
C21 C22 1.362(7) yes .
C22 C23 1.377(7) yes .
C23 C24 1.394(5) yes .
C25 C26 1.394(5) yes .
C25 C30 1.397(5) yes .
C26 C27 1.385(5) yes .
C27 C28 1.374(5) yes .
C28 C29 1.385(5) yes .
C29 C30 1.388(5) yes .
C31 C32 1.377(8) yes .
C32 C33 1.375(10) yes .
C33 C34 1.358(8) yes .
C34 C35 1.368(8) yes .
