#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:37:02 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179338 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/35/4323505.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_4323505
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            'C26 H30 Cl2 N6 P2 Re'
_chemical_formula_weight         745.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.383(4)
_cell_length_b                   13.967(3)
_cell_length_c                   12.002(2)
_cell_measurement_temperature    296(2)
_cell_volume                     2913.9(10)
_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      296(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  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            11285
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    4.490
_exptl_absorpt_correction_T_max  0.2934
_exptl_absorpt_correction_T_min  0.2227
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          .32
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .28
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.190
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(12)
_refine_ls_extinction_coef       0.0023(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.227
_refine_ls_goodness_of_fit_obs   1.044
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         3083
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.226
_refine_ls_restrained_S_obs      1.043
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_obs          0.0281
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0479P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0840
_refine_ls_wR_factor_obs         0.0673
_reflns_number_observed          2773
_reflns_number_total             3083
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961489t_2.cif
_cod_data_source_block           psi1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+0.0000P] 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^)+(0.0479P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323505
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, 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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Re Re 0.16450(2) 0.14389(2) 0.25184(7) 0.0313(2) Uani 1 d . .
Cl1 Cl 0.2414(2) 0.1704(2) 0.0870(2) 0.0454(7) Uani 1 d . .
P1 P 0.0758(2) 0.0610(2) 0.1265(2) 0.0381(6) Uani 1 d . .
P2 P 0.2648(2) 0.2313(2) 0.3534(3) 0.0383(7) Uani 1 d . .
N11 N 0.1031(4) 0.2478(5) 0.2528(11) 0.038(2) Uani 1 d . .
N12 N 0.0564(4) 0.3124(5) 0.2636(11) 0.041(2) Uani 1 d . .
N13 N 0.0013(5) 0.4553(6) 0.2100(9) 0.058(3) Uani 1 d . .
N21 N 0.2218(4) 0.0084(5) 0.2817(6) 0.033(2) Uani 1 d . .
N22 N 0.1238(5) 0.0936(5) 0.3914(8) 0.040(2) Uani 1 d . .
N23 N 0.1436(6) 0.0126(6) 0.4399(8) 0.049(2) Uani 1 d . .
C11 C 0.0346(6) 0.1404(7) 0.0220(10) 0.040(3) Uani 1 d . .
C12 C 0.0647(7) 0.1515(8) -0.0830(11) 0.057(4) Uani 1 d . .
H12B H 0.1068(7) 0.1150(8) -0.1049(11) 0.069 Uiso 1 calc R .
C13 C 0.0325(10) 0.2173(11) -0.1571(12) 0.076(5) Uani 1 d . .
H13B H 0.0531(10) 0.2235(11) -0.2282(12) 0.092 Uiso 1 calc R .
C14 C -0.0277(9) 0.2717(11) -0.1276(17) 0.081(5) Uani 1 d . .
H14A H -0.0485(9) 0.3150(11) -0.1782(17) 0.097 Uiso 1 calc R .
C15 C -0.0588(8) 0.2637(10) -0.0226(16) 0.078(5) Uani 1 d . .
H15A H -0.1001(8) 0.3020(10) -0.0015(16) 0.094 Uiso 1 calc R .
C16 C -0.0282(7) 0.1982(8) 0.0506(12) 0.059(3) Uani 1 d . .
H16A H -0.0498(7) 0.1922(8) 0.1212(12) 0.071 Uiso 1 calc R .
C17 C -0.0062(6) 0.0118(9) 0.1992(11) 0.062(3) Uani 1 d . .
H17A H 0.0113(6) -0.0312(9) 0.2562(11) 0.074 Uiso 1 calc R .
H17B H -0.0382(6) -0.0222(9) 0.1475(11) 0.074 Uiso 1 calc R .
H17C H -0.0351(6) 0.0629(9) 0.2326(11) 0.074 Uiso 1 calc R .
C18 C 0.1164(8) -0.0388(8) 0.0481(14) 0.070(4) Uani 1 d . .
H18A H 0.1606(8) -0.0173(8) 0.0072(14) 0.083 Uiso 1 calc R .
H18B H 0.0785(8) -0.0631(8) -0.0028(14) 0.083 Uiso 1 calc R .
H18C H 0.1314(8) -0.0887(8) 0.0987(14) 0.083 Uiso 1 calc R .
C21 C 0.2503(6) 0.3603(6) 0.3364(10) 0.041(3) Uani 1 d . .
C22 C 0.2893(6) 0.4105(7) 0.2561(17) 0.055(3) Uani 1 d . .
H22B H 0.3268(6) 0.3806(7) 0.2133(17) 0.066 Uiso 1 calc R .
C23 C 0.2719(7) 0.5083(8) 0.2391(17) 0.071(4) Uani 1 d . .
H23B H 0.2991(7) 0.5436(8) 0.1865(17) 0.085 Uiso 1 calc R .
C24 C 0.2150(8) 0.5509(9) 0.3005(15) 0.081(6) Uani 1 d . .
H24A H 0.2039(8) 0.6154(9) 0.2895(15) 0.097 Uiso 1 calc R .
C25 C 0.1745(7) 0.4997(9) 0.3776(13) 0.063(4) Uani 1 d . .
H25A H 0.1349(7) 0.5285(9) 0.4174(13) 0.075 Uiso 1 calc R .
C26 C 0.1928(7) 0.4043(8) 0.3963(11) 0.049(3) Uani 1 d . .
H26A H 0.1659(7) 0.3698(8) 0.4500(11) 0.058 Uiso 1 calc R .
C27 C 0.3623(6) 0.2042(8) 0.3113(12) 0.058(3) Uani 1 d . .
H27A H 0.3675(6) 0.2142(8) 0.2326(12) 0.070 Uiso 1 calc R .
H27B H 0.3737(6) 0.1386(8) 0.3287(12) 0.070 Uiso 1 calc R .
H27C H 0.3974(6) 0.2453(8) 0.3504(12) 0.070 Uiso 1 calc R .
C28 C 0.2656(7) 0.2089(8) 0.5015(11) 0.060(3) Uani 1 d . .
H28A H 0.2155(7) 0.2216(8) 0.5317(11) 0.072 Uiso 1 calc R .
H28B H 0.3027(7) 0.2499(8) 0.5366(11) 0.072 Uiso 1 calc R .
H28C H 0.2789(7) 0.1432(8) 0.5150(11) 0.072 Uiso 1 calc R .
C111 C 0.0542(6) 0.3879(7) 0.1827(10) 0.038(3) Uani 1 d . .
C112 C 0.0987(7) 0.3918(8) 0.0910(11) 0.050(3) Uani 1 d . .
H11A H 0.1351(7) 0.3444(8) 0.0769(11) 0.061 Uiso 1 calc R .
C113 C 0.0893(8) 0.4672(8) 0.0186(12) 0.072(4) Uani 1 d . .
H11B H 0.1197(8) 0.4713(8) -0.0449(12) 0.087 Uiso 1 calc R .
C114 C 0.0363(7) 0.5349(8) 0.0395(14) 0.067(4) Uani 1 d . .
H11C H 0.0270(7) 0.5843(8) -0.0108(14) 0.081 Uiso 1 calc R .
C115 C -0.0033(7) 0.5284(9) 0.1367(16) 0.079(5) Uani 1 d . .
H11D H -0.0363(7) 0.5785(9) 0.1544(16) 0.095 Uiso 1 calc R .
C211 C 0.1971(5) -0.0358(7) 0.3757(9) 0.035(2) Uani 1 d . .
C212 C 0.2241(6) -0.1258(7) 0.4082(12) 0.047(3) Uani 1 d . .
H21A H 0.2070(6) -0.1538(7) 0.4740(12) 0.056 Uiso 1 calc R .
C213 C 0.2746(6) -0.1709(8) 0.3436(12) 0.051(3) Uani 1 d . .
H21B H 0.2926(6) -0.2312(8) 0.3634(12) 0.061 Uiso 1 calc R .
C214 C 0.3004(6) -0.1273(6) 0.2462(21) 0.055(3) Uani 1 d . .
H21C H 0.3347(6) -0.1590(6) 0.1996(21) 0.066 Uiso 1 calc R .
C215 C 0.2750(5) -0.0376(7) 0.2194(9) 0.043(3) Uani 1 d . .
H21D H 0.2949(5) -0.0074(7) 0.1567(9) 0.052 Uiso 1 calc R .
Cl2 Cl 0.0466(3) 0.2297(2) 0.5492(3) 0.0756(11) Uani 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'
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 -1.0185 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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N11 Re N22 94.0(4) . . ?
N11 Re N21 166.9(4) . . ?
N22 Re N21 73.2(3) . . ?
N11 Re Cl1 102.1(4) . . ?
N22 Re Cl1 163.7(2) . . ?
N21 Re Cl1 90.8(2) . . ?
N11 Re P1 90.7(3) . . ?
N22 Re P1 97.4(3) . . ?
N21 Re P1 88.7(2) . . ?
Cl1 Re P1 85.26(10) . . ?
N11 Re P2 91.0(3) . . ?
N22 Re P2 90.6(3) . . ?
N21 Re P2 91.5(2) . . ?
Cl1 Re P2 86.40(10) . . ?
P1 Re P2 171.66(10) . . ?
C17 P1 C11 104.7(5) . . ?
C17 P1 C18 105.3(6) . . ?
C11 P1 C18 105.2(6) . . ?
C17 P1 Re 112.3(4) . . ?
C11 P1 Re 112.5(3) . . ?
C18 P1 Re 115.8(5) . . ?
C27 P2 C28 103.4(6) . . ?
C27 P2 C21 107.7(5) . . ?
C28 P2 C21 106.3(6) . . ?
C27 P2 Re 115.1(4) . . ?
C28 P2 Re 114.1(4) . . ?
C21 P2 Re 109.6(3) . . ?
N12 N11 Re 172.0(9) . . ?
N11 N12 C111 119.3(11) . . ?
C115 N13 C111 114.1(11) . . ?
C215 N21 C211 117.3(8) . . ?
C215 N21 Re 129.7(6) . . ?
C211 N21 Re 113.0(6) . . ?
N23 N22 Re 126.4(7) . . ?
N22 N23 C211 110.4(9) . . ?
C12 C11 C16 117.2(12) . . ?
C12 C11 P1 123.4(9) . . ?
C16 C11 P1 119.3(10) . . ?
C11 C12 C13 120.3(12) . . ?
C14 C13 C12 121.3(14) . . ?
C13 C14 C15 120.1(15) . . ?
C16 C15 C14 119.2(15) . . ?
C15 C16 C11 121.9(14) . . ?
C22 C21 C26 119.8(10) . . ?
C22 C21 P2 120.9(9) . . ?
C26 C21 P2 118.8(9) . . ?
C21 C22 C23 119.4(14) . . ?
C24 C23 C22 119.8(15) . . ?
C25 C24 C23 120.6(12) . . ?
C24 C25 C26 119.6(13) . . ?
C21 C26 C25 120.7(12) . . ?
C112 C111 N13 124.0(10) . . ?
C112 C111 N12 124.6(9) . . ?
N13 C111 N12 111.4(10) . . ?
C111 C112 C113 118.6(11) . . ?
C114 C113 C112 120.2(13) . . ?
C113 C114 C115 117.4(12) . . ?
N13 C115 C114 125.5(11) . . ?
N21 C211 N23 116.9(8) . . ?
N21 C211 C212 122.4(10) . . ?
N23 C211 C212 120.6(10) . . ?
C213 C212 C211 119.0(12) . . ?
C212 C213 C214 119.7(11) . . ?
C215 C214 C213 119.6(14) . . ?
N21 C215 C214 121.8(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 N11 1.802(7) . ?
Re N22 1.949(9) . ?
Re N21 2.167(7) . ?
Re Cl1 2.416(3) . ?
Re P1 2.445(3) . ?
Re P2 2.453(3) . ?
P1 C17 1.807(11) . ?
P1 C11 1.822(11) . ?
P1 C18 1.823(12) . ?
P2 C27 1.808(11) . ?
P2 C28 1.805(13) . ?
P2 C21 1.830(9) . ?
N11 N12 1.221(9) . ?
N12 C111 1.43(2) . ?
N13 C115 1.35(2) . ?
N13 C111 1.357(13) . ?
N21 C215 1.352(12) . ?
N21 C211 1.356(13) . ?
N22 N23 1.319(11) . ?
N23 C211 1.384(13) . ?
C11 C12 1.37(2) . ?
C11 C16 1.400(15) . ?
C12 C13 1.40(2) . ?
C13 C14 1.34(2) . ?
C14 C15 1.38(2) . ?
C15 C16 1.38(2) . ?
C21 C22 1.37(2) . ?
C21 C26 1.38(2) . ?
C22 C23 1.41(2) . ?
C23 C24 1.37(2) . ?
C24 C25 1.37(2) . ?
C25 C26 1.39(2) . ?
C111 C112 1.35(2) . ?
C112 C113 1.37(2) . ?
C113 C114 1.34(2) . ?
C114 C115 1.36(2) . ?
C211 C212 1.397(14) . ?
C212 C213 1.33(2) . ?
C213 C214 1.39(2) . ?
C214 C215 1.367(14) . ?
