#------------------------------------------------------------------------------
#$Date: 2025-08-21 01:01:10 +0300 (Thu, 21 Aug 2025) $
#$Revision: 301838 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/35/4323504.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_4323504
loop_
_publ_author_name
'Melissa Hirsch-Kuchma'
'Terrence Nicholson'
'Alan Davison'
'William M. Davis'
'Alun G. Jones'
_publ_section_title
;
 Synthesis and Characterization of Rhenium(III) and Technetium(III)
 Organohydrazide Chelate Complexes. Reactions of 2-Hydrazinopyridine with
 Complexes of Rhenium and Technetium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3237
_journal_page_last               3241
_journal_paper_doi               10.1021/ic961489t
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C41.5 H34 Cl2 N3 O0.5 P2 Re'
_chemical_formula_weight         901.76
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                105.9050(10)
_cell_angle_beta                 95.8930(10)
_cell_angle_gamma                111.0100(10)
_cell_formula_units_Z            2
_cell_length_a                   10.5549(7)
_cell_length_b                   12.2699(8)
_cell_length_c                   16.8206(12)
_cell_measurement_temperature    188(2)
_cell_volume                     1906.1(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      188(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω 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  0.0920
_diffrn_reflns_av_sigmaI/netI    0.0651
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7684
_diffrn_reflns_theta_max         23.34
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    3.322
_exptl_absorpt_correction_T_max  0.6355
_exptl_absorpt_correction_T_min  0.4050
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             894
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.959
_refine_diff_density_min         -2.097
_refine_diff_density_rms         0.256
_refine_ls_extinction_coef       0.0082(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.223
_refine_ls_goodness_of_fit_obs   1.179
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         5268
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.319
_refine_ls_restrained_S_obs      1.179
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_obs          0.0496
_refine_ls_shift/esd_max         -0.022
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0908P)²+9.5106P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1713
_refine_ls_wR_factor_obs         0.1454
_reflns_number_observed          4792
_reflns_number_total             5273
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961489t_1.cif
_cod_data_source_block           copy
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0908P)^2^+9.5106P] 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^)+(0.0908P)^2^+9.5106P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C41.50 H34 Cl2 N3 O0.50 P2 Re'
_cod_database_code               4323504
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Re Re 0.28643(3) 0.20456(3) 0.22219(2) 0.0243(2) Uani 1 d . .
Cl2 Cl 0.1789(3) 0.0125(2) 0.10880(15) 0.0343(6) Uani 1 d . .
Cl1 Cl 0.5051(3) 0.1908(3) 0.2512(2) 0.0403(6) Uani 1 d . .
P1 P 0.3818(2) 0.3222(2) 0.1296(2) 0.0261(5) Uani 1 d . .
P2 P 0.2132(3) 0.0941(2) 0.3233(2) 0.0285(6) Uani 1 d . .
N3 N 0.0879(8) 0.2182(7) 0.1947(5) 0.028(2) Uani 1 d . .
N1 N 0.2889(8) 0.3435(7) 0.2977(5) 0.028(2) Uani 1 d . .
N2 N 0.2037(9) 0.3909(9) 0.3162(5) 0.040(2) Uani 1 d . .
C21 C 0.0511(11) 0.0982(9) 0.3503(7) 0.033(2) Uani 1 d . .
C1 C 0.0813(10) 0.3170(8) 0.2545(6) 0.029(2) Uani 1 d . .
C41 C 0.4941(10) 0.4827(10) 0.1889(6) 0.033(2) Uani 1 d . .
C51 C 0.4884(10) 0.2724(11) 0.0604(6) 0.036(2) Uani 1 d . .
C46 C 0.5879(11) 0.5096(11) 0.2639(7) 0.043(3) Uani 1 d . .
H46A H 0.5869(11) 0.4447(11) 0.2845(7) 0.052 Uiso 1 calc R .
C42 C 0.4991(11) 0.5808(10) 0.1602(7) 0.040(2) Uani 1 d . .
H42A H 0.4384(11) 0.5643(10) 0.1086(7) 0.048 Uiso 1 calc R .
C52 C 0.6089(11) 0.3596(11) 0.0504(7) 0.040(2) Uani 1 d . .
H52A H 0.6397(11) 0.4451(11) 0.0820(7) 0.048 Uiso 1 calc R .
C41 C 0.1705(11) 0.3940(12) 0.0897(7) 0.043(3) Uani 1 d . .
H41A H 0.1896(11) 0.4334(12) 0.1493(7) 0.052 Uiso 1 calc R .
C5 C -0.0354(12) 0.3428(12) 0.2516(8) 0.048(3) Uani 1 d . .
H5A H -0.0379(12) 0.4104(12) 0.2946(8) 0.058 Uiso 1 calc R .
C11 C 0.2499(10) 0.3351(11) 0.0568(6) 0.038(3) Uani 1 d . .
C3 C -0.1406(11) 0.1736(12) 0.1214(7) 0.046(3) Uani 1 d . .
H3A H -0.2157(11) 0.1251(12) 0.0734(7) 0.056 Uiso 1 calc R .
C31 C 0.3408(11) 0.1607(10) 0.4242(6) 0.035(2) Uani 1 d . .
C22 C -0.0668(11) 0.0439(10) 0.2867(8) 0.041(3) Uani 1 d . .
H22A H -0.0649(11) -0.0021(10) 0.2316(8) 0.049 Uiso 1 calc R .
C66 C 0.2788(12) -0.1080(11) 0.2610(7) 0.041(3) Uani 1 d . .
H66A H 0.3538(12) -0.0513(11) 0.2467(7) 0.049 Uiso 1 calc R .
C61 C 0.1828(10) -0.0692(9) 0.2961(6) 0.030(2) Uani 1 d . .
C54 C 0.6392(13) 0.1991(13) -0.0529(8) 0.049(3) Uani 1 d . .
H54A H 0.6913(13) 0.1734(13) -0.0911(8) 0.059 Uiso 1 calc R .
C53 C 0.6830(12) 0.3200(12) -0.0061(8) 0.048(3) Uani 1 d . .
H53A H 0.7661(12) 0.3788(12) -0.0120(8) 0.058 Uiso 1 calc R .
C56 C 0.4451(12) 0.1488(11) 0.0127(7) 0.046(3) Uani 1 d . .
H56A H 0.3646(12) 0.0884(11) 0.0197(7) 0.055 Uiso 1 calc R .
C62 C 0.0724(12) -0.1542(11) 0.3145(8) 0.045(3) Uani 1 d . .
H62A H 0.0055(12) -0.1292(11) 0.3385(8) 0.054 Uiso 1 calc R .
C6 C -0.0230(10) 0.1501(10) 0.1283(6) 0.037(2) Uani 1 d . .
H6A H -0.0193(10) 0.0836(10) 0.0849(6) 0.044 Uiso 1 calc R .
C55 C 0.5184(15) 0.1132(13) -0.0449(8) 0.055(3) Uani 1 d . .
H55A H 0.4855(15) 0.0288(13) -0.0795(8) 0.066 Uiso 1 calc R .
C42 C 0.0628(12) 0.3979(10) 0.0385(8) 0.044(3) Uani 1 d . .
H42B H 0.0099(12) 0.4411(10) 0.0631(8) 0.052 Uiso 1 calc R .
C63 C 0.0588(13) -0.2729(11) 0.2987(8) 0.052(3) Uani 1 d . .
H63A H -0.0186(13) -0.3302(11) 0.3107(8) 0.062 Uiso 1 calc R .
C43 C 0.0313(12) 0.3405(12) -0.0472(8) 0.053(3) Uani 1 d . .
H43A H -0.0431(12) 0.3432(12) -0.0824(8) 0.064 Uiso 1 calc R .
C42 C 0.6829(12) 0.6310(12) 0.3087(8) 0.055(3) Uani 1 d . .
H42C H 0.7474(12) 0.6487(12) 0.3591(8) 0.066 Uiso 1 calc R .
C4 C -0.1491(12) 0.2679(13) 0.1847(8) 0.052(3) Uani 1 d . .
H4A H -0.2323(12) 0.2815(13) 0.1823(8) 0.063 Uiso 1 calc R .
C13 C 0.1098(14) 0.2779(12) -0.0821(8) 0.053(3) Uani 1 d . .
H13A H 0.0893(14) 0.2386(12) -0.1418(8) 0.064 Uiso 1 calc R .
C12 C 0.2193(12) 0.2714(12) -0.0308(7) 0.049(3) Uani 1 d . .
H12A H 0.2705(12) 0.2258(12) -0.0545(7) 0.058 Uiso 1 calc R .
C44 C 0.5915(12) 0.7018(11) 0.2060(9) 0.052(3) Uani 1 d . .
H44A H 0.5916(12) 0.7678(11) 0.1868(9) 0.063 Uiso 1 calc R .
C23 C -0.1897(13) 0.0556(12) 0.3019(9) 0.053(3) Uani 1 d . .
H23A H -0.2693(13) 0.0202(12) 0.2566(9) 0.064 Uiso 1 calc R .
C34 C 0.5385(16) 0.2720(16) 0.5762(8) 0.072(4) Uani 1 d . .
H34A H 0.6069(16) 0.3094(16) 0.6279(8) 0.086 Uiso 1 calc R .
C35 C 0.4666(21) 0.1479(16) 0.5454(10) 0.089(6) Uani 1 d . .
H35A H 0.4833(21) 0.0992(16) 0.5771(10) 0.107 Uiso 1 calc R .
C45 C 0.6819(12) 0.7254(11) 0.2787(9) 0.054(3) Uani 1 d . .
H45A H 0.7456(12) 0.8082(11) 0.3094(9) 0.064 Uiso 1 calc R .
C36 C 0.3695(17) 0.0895(13) 0.4692(9) 0.070(4) Uani 1 d . .
H36A H 0.3229(17) 0.0018(13) 0.4478(9) 0.084 Uiso 1 calc R .
C26 C 0.0424(16) 0.1638(14) 0.4303(9) 0.065(4) Uani 1 d . .
H26A H 0.1222(16) 0.2043(14) 0.4759(9) 0.078 Uiso 1 calc R .
C32 C 0.4144(16) 0.2876(13) 0.4571(8) 0.074(5) Uani 1 d . .
H32A H 0.3967(16) 0.3374(13) 0.4267(8) 0.089 Uiso 1 calc R .
C25 C -0.0828(18) 0.1694(18) 0.4428(11) 0.086(5) Uani 1 d . .
H25A H -0.0887(18) 0.2122(18) 0.4978(11) 0.103 Uiso 1 calc R .
C24 C -0.1965(16) 0.1157(17) 0.3790(12) 0.079(5) Uani 1 d . .
H24A H -0.2816(16) 0.1207(17) 0.3890(12) 0.095 Uiso 1 calc R .
C33 C 0.5122(19) 0.3443(15) 0.5324(9) 0.088(6) Uani 1 d . .
H33A H 0.5610(19) 0.4319(15) 0.5539(9) 0.106 Uiso 1 calc R .
C64 C 0.1572(14) -0.3121(10) 0.2648(7) 0.048(3) Uani 1 d . .
H64A H 0.1480(14) -0.3949(10) 0.2549(7) 0.057 Uiso 1 calc R .
C65 C 0.2669(13) -0.2290(12) 0.2463(7) 0.049(3) Uani 1 d . .
H65A H 0.3348(13) -0.2539(12) 0.2235(7) 0.059 Uiso 1 calc R .
C7 C 0.1211(47) 0.5257(36) 0.4890(34) 0.153(25) Uani 0.50 d P .
O7 O 0.1752(34) 0.5132(30) 0.5653(14) 0.153(17) Uani 0.50 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'
P P 0.1023 0.0942 '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'
Re Re -1.5980 7.2320 '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'
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
N1 Re N3 69.9(3) . . ?
N1 Re Cl2 154.3(3) . . ?
N3 Re Cl2 84.6(2) . . ?
N1 Re Cl1 110.1(3) . . ?
N3 Re Cl1 179.3(2) . . ?
Cl2 Re Cl1 95.40(9) . . ?
N1 Re P1 90.3(2) . . ?
N3 Re P1 91.7(2) . . ?
Cl2 Re P1 93.65(8) . . ?
Cl1 Re P1 87.67(8) . . ?
N1 Re P2 88.9(2) . . ?
N3 Re P2 93.1(2) . . ?
Cl2 Re P2 89.41(8) . . ?
Cl1 Re P2 87.61(9) . . ?
P1 Re P2 174.59(8) . . ?
C41 P1 C51 102.9(5) . . ?
C41 P1 C11 102.8(5) . . ?
C51 P1 C11 103.5(5) . . ?
C41 P1 Re 112.3(3) . . ?
C51 P1 Re 119.2(4) . . ?
C11 P1 Re 114.3(3) . . ?
C61 P2 C21 103.7(4) . . ?
C61 P2 C31 100.9(4) . . ?
C21 P2 C31 105.7(5) . . ?
C61 P2 Re 120.0(3) . . ?
C21 P2 Re 111.9(3) . . ?
C31 P2 Re 113.0(3) . . ?
C6 N3 C1 117.2(9) . . ?
C6 N3 Re 130.7(7) . . ?
C1 N3 Re 112.0(6) . . ?
N2 N1 Re 137.3(7) . . ?
N1 N2 C1 105.8(8) . . ?
C22 C21 C26 117.4(11) . . ?
C22 C21 P2 118.4(8) . . ?
C26 C21 P2 123.9(10) . . ?
N3 C1 N2 114.5(8) . . ?
N3 C1 C5 122.6(10) . . ?
N2 C1 C5 122.9(9) . . ?
C46 C41 C42 118.0(10) . . ?
C46 C41 P1 118.7(8) . . ?
C42 C41 P1 123.2(8) . . ?
C56 C51 C52 119.1(9) . . ?
C56 C51 P1 120.2(8) . . ?
C52 C51 P1 120.5(9) . . ?
C42 C46 C41 120.7(11) . . ?
C44 C42 C41 121.2(11) . . ?
C51 C52 C53 119.3(11) . . ?
C11 C41 C42 121.3(11) . . ?
C4 C5 C1 118.5(11) . . ?
C41 C11 C12 120.2(10) . . ?
C41 C11 P1 118.8(8) . . ?
C12 C11 P1 120.5(9) . . ?
C4 C3 C6 119.6(11) . . ?
C36 C31 C32 117.9(10) . . ?
C36 C31 P2 123.2(9) . . ?
C32 C31 P2 118.9(8) . . ?
C23 C22 C21 120.7(12) . . ?
C61 C66 C65 120.8(10) . . ?
C62 C61 C66 118.6(10) . . ?
C62 C61 P2 122.5(8) . . ?
C66 C61 P2 118.7(8) . . ?
C55 C54 C53 119.8(10) . . ?
C54 C53 C52 121.1(11) . . ?
C55 C56 C51 120.2(11) . . ?
C63 C62 C61 120.8(11) . . ?
N3 C6 C3 122.4(10) . . ?
C54 C55 C56 120.5(12) . . ?
C41 C42 C43 120.7(11) . . ?
C62 C63 C64 121.0(11) . . ?
C42 C43 C13 118.9(10) . . ?
C45 C42 C46 119.1(12) . . ?
C3 C4 C5 119.5(10) . . ?
C43 C13 C12 121.4(11) . . ?
C13 C12 C11 117.4(11) . . ?
C45 C44 C42 119.6(11) . . ?
C24 C23 C22 120.8(14) . . ?
C35 C34 C33 119.7(13) . . ?
C34 C35 C36 122.0(14) . . ?
C44 C45 C42 121.4(11) . . ?
C31 C36 C35 119.3(14) . . ?
C21 C26 C25 119.7(14) . . ?
C33 C32 C31 122.2(13) . . ?
C24 C25 C26 121.5(14) . . ?
C23 C24 C25 119.8(13) . . ?
C34 C33 C32 118.9(15) . . ?
C65 C64 C63 118.9(10) . . ?
C64 C65 C66 119.9(11) . . ?
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 N1 1.815(8) . ?
Re N3 2.174(8) . ?
Re Cl2 2.378(2) . ?
Re Cl1 2.385(2) . ?
Re P1 2.457(2) . ?
Re P2 2.472(2) . ?
P1 C41 1.812(10) . ?
P1 C51 1.835(10) . ?
P1 C11 1.837(10) . ?
P2 C61 1.825(10) . ?
P2 C21 1.829(10) . ?
P2 C31 1.828(10) . ?
N3 C6 1.355(13) . ?
N3 C1 1.375(12) . ?
N1 N2 1.256(12) . ?
N2 C1 1.391(14) . ?
C21 C22 1.37(2) . ?
C21 C26 1.40(2) . ?
C1 C5 1.378(15) . ?
C41 C46 1.40(2) . ?
C41 C42 1.400(15) . ?
C51 C56 1.38(2) . ?
C51 C52 1.400(15) . ?
C46 C42 1.40(2) . ?
C42 C44 1.39(2) . ?
C52 C53 1.39(2) . ?
C41 C11 1.36(2) . ?
C41 C42 1.38(2) . ?
C5 C4 1.38(2) . ?
C11 C12 1.41(2) . ?
C3 C4 1.38(2) . ?
C3 C6 1.37(2) . ?
C31 C36 1.39(2) . ?
C31 C32 1.38(2) . ?
C22 C23 1.40(2) . ?
C66 C61 1.385(15) . ?
C66 C65 1.39(2) . ?
C61 C62 1.386(15) . ?
C54 C55 1.38(2) . ?
C54 C53 1.35(2) . ?
C56 C55 1.37(2) . ?
C62 C63 1.36(2) . ?
C42 C43 1.36(2) . ?
C63 C64 1.40(2) . ?
C43 C13 1.39(2) . ?
C42 C45 1.39(2) . ?
C13 C12 1.41(2) . ?
C44 C45 1.36(2) . ?
C23 C24 1.33(2) . ?
C34 C35 1.35(2) . ?
C34 C33 1.38(2) . ?
C35 C36 1.38(2) . ?
C26 C25 1.38(2) . ?
C32 C33 1.37(2) . ?
C25 C24 1.35(2) . ?
C64 C65 1.37(2) . ?
C7 O7 1.42(6) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139135056
