#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/21/7012172.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_7012172
loop_
_publ_author_name
'Chakraborty, Indranil'
'Sengupta, Suman'
'Das, Samir'
'Banerjee, Sangeeta'
'Chakravorty, Animesh'
_publ_section_title
;
 Chemistry of monovalent and bivalent rhenium: synthesis, structure,
 isomer specificity and metal redox of azoheterocycle complexes
;
_journal_issue                   1
_journal_name_full               'Dalton Transactions'
_journal_page_first              134
_journal_paper_doi               10.1039/b208338h
_journal_year                    2003
_chemical_formula_sum            'C34 H32 I2 N8 Re'
_chemical_formula_weight         992.68
_chemical_name_systematic
; 
? 
;
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 99.60(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.946(2)
_cell_length_b                   18.790(4)
_cell_length_c                   17.394(4)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7
_cell_volume                     3527.4(13)
_computing_cell_refinement       'Siemens P3/P4-PC V4.27'
_computing_data_collection       'Siemens P3/P4-PC V4.27'
_computing_data_reduction        'Siemens P3/P4-PC V4.27'
_computing_molecular_graphics    'Siemens SHELXTL V5.03 PC'
_computing_publication_material  'Siemens SHELXTL V5.03 PC'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3m/V'
_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  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0630
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5684
_diffrn_reflns_theta_max         23.55
_diffrn_reflns_theta_min         1.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    5.231
_exptl_absorpt_correction_T_max  0.254
_exptl_absorpt_correction_T_min  0.195
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_description       parallelopiped
_exptl_crystal_F_000             1892
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.031
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.044
_refine_ls_goodness_of_fit_obs   1.093
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5255
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_restrained_S_obs      1.093
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_obs          0.0483
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0482P)²+6.8352P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1206
_refine_ls_wR_factor_obs         0.0955
_reflns_number_observed          3631
_reflns_number_total             5257
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b208338h.txt
_cod_data_source_block           647re
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+6.8352P] 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^)+(0.0482P)^2^+6.8352P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Heavy atom method' was changed
to 'heavy'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        3527.4(12)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7012172
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Re Re 0.86780(4) 0.15984(2) 0.15158(3) 0.0433(2) Uani 1 d . .
I2 I 0.68059(7) 0.07996(4) 0.06952(5) 0.0616(3) Uani 1 d . .
I1 I 0.92174(10) 0.06727(5) 0.27282(5) 0.0839(3) Uani 1 d . .
N1 N 0.9956(7) 0.1072(4) 0.0974(5) 0.044(2) Uani 1 d . .
N2 N 1.0854(9) 0.0974(5) -0.0069(6) 0.056(3) Uani 1 d . .
N3 N 0.9481(8) 0.1956(4) 0.0013(5) 0.043(2) Uani 1 d . .
N4 N 0.8803(8) 0.2178(4) 0.0540(5) 0.043(2) Uani 1 d . .
N5 N 0.7386(7) 0.2048(4) 0.2098(5) 0.043(2) Uani 1 d . .
N6 N 0.7034(9) 0.2805(5) 0.3023(5) 0.054(2) Uani 1 d . .
N7 N 0.9010(8) 0.2815(5) 0.2600(5) 0.047(2) Uani 1 d . .
N8 N 0.9570(8) 0.2411(5) 0.2106(5) 0.046(2) Uani 1 d . .
C1 C 1.0737(11) 0.0503(6) 0.1076(7) 0.060(3) Uani 1 d . .
H1A H 1.0879(11) 0.0206(6) 0.1509(7) 0.072 Uiso 1 calc R .
C2 C 1.1271(12) 0.0450(7) 0.0425(8) 0.066(4) Uani 1 d . .
H2A H 1.1837(12) 0.0103(7) 0.0338(8) 0.079 Uiso 1 calc R .
C3 C 1.0060(10) 0.1354(6) 0.0282(6) 0.046(3) Uani 1 d . .
C4 C 0.8357(9) 0.2890(5) 0.0386(6) 0.038(2) Uani 1 d . .
C5 C 0.9084(12) 0.3360(6) 0.0048(7) 0.070(4) Uani 1 d . .
H5A H 0.9838(12) 0.3216(6) -0.0079(7) 0.084 Uiso 1 calc R .
C6 C 0.8655(16) 0.4054(7) -0.0098(8) 0.095(5) Uani 1 d . .
H6A H 0.9099(16) 0.4366(7) -0.0362(8) 0.114 Uiso 1 calc R .
C7 C 0.7609(16) 0.4281(7) 0.0137(9) 0.090(5) Uani 1 d . .
C8 C 0.6900(13) 0.3809(6) 0.0477(8) 0.076(4) Uani 1 d . .
H8A H 0.6157(13) 0.3958(6) 0.0618(8) 0.091 Uiso 1 calc R .
C9 C 0.7294(11) 0.3110(6) 0.0609(7) 0.057(3) Uani 1 d . .
H9A H 0.6827(11) 0.2794(6) 0.0852(7) 0.068 Uiso 1 calc R .
C10 C 0.7106(20) 0.5036(8) -0.0052(11) 0.164(10) Uani 1 d . .
H10A H 0.6360(20) 0.5101(8) 0.0162(11) 0.246 Uiso 1 calc R .
H10B H 0.6930(20) 0.5099(8) -0.0607(11) 0.246 Uiso 1 calc R .
H10C H 0.7713(20) 0.5379(8) 0.0172(11) 0.246 Uiso 1 calc R .
C11 C 1.1246(11) 0.1146(6) -0.0812(6) 0.062(3) Uani 1 d . .
H11A H 1.0523(11) 0.1268(6) -0.1191(6) 0.075 Uiso 1 calc R .
H11B H 1.1622(11) 0.0728(6) -0.1001(6) 0.075 Uiso 1 calc R .
C12 C 1.2153(11) 0.1751(6) -0.0748(6) 0.048(3) Uani 1 d . .
C13 C 1.1770(13) 0.2411(8) -0.1021(7) 0.073(4) Uani 1 d . .
H13A H 1.0944(13) 0.2493(8) -0.1233(7) 0.088 Uiso 1 calc R .
C14 C 1.2623(17) 0.2952(8) -0.0978(9) 0.089(4) Uani 1 d . .
H14A H 1.2365(17) 0.3399(8) -0.1172(9) 0.106 Uiso 1 calc R .
C15 C 1.3838(17) 0.2854(10) -0.0660(9) 0.091(5) Uani 1 d . .
H15A H 1.4395(17) 0.3230(10) -0.0636(9) 0.110 Uiso 1 calc R .
C16 C 1.4232(14) 0.2202(11) -0.0375(9) 0.091(5) Uani 1 d . .
H16A H 1.5056(14) 0.2133(11) -0.0151(9) 0.109 Uiso 1 calc R .
C17 C 1.3387(13) 0.1635(8) -0.0421(8) 0.080(4) Uani 1 d . .
H17A H 1.3648(13) 0.1186(8) -0.0236(8) 0.095 Uiso 1 calc R .
C18 C 0.5996(12) 0.2410(7) 0.2797(7) 0.063(3) Uani 1 d . .
H18A H 0.5258(12) 0.2455(7) 0.2991(7) 0.075 Uiso 1 calc R .
C19 C 0.6205(10) 0.1942(6) 0.2248(7) 0.054(3) Uani 1 d . .
H19A H 0.5646(10) 0.1604(6) 0.2010(7) 0.065 Uiso 1 calc R .
C20 C 0.7880(10) 0.2572(6) 0.2590(6) 0.047(3) Uani 1 d . .
C21 C 1.0721(11) 0.2698(6) 0.1982(6) 0.051(3) Uani 1 d . .
C22 C 1.1658(10) 0.2244(6) 0.1862(6) 0.056(3) Uani 1 d . .
H22A H 1.1558(10) 0.1754(6) 0.1902(6) 0.068 Uiso 1 calc R .
C23 C 1.2739(11) 0.2516(8) 0.1684(7) 0.066(4) Uani 1 d . .
H23A H 1.3363(11) 0.2204(8) 0.1599(7) 0.080 Uiso 1 calc R .
C24 C 1.2922(11) 0.3225(8) 0.1628(7) 0.063(4) Uani 1 d . .
C25 C 1.1994(12) 0.3682(7) 0.1787(7) 0.062(3) Uani 1 d . .
H25A H 1.2123(12) 0.4171(7) 0.1781(7) 0.074 Uiso 1 calc R .
C26 C 1.0892(11) 0.3425(7) 0.1954(7) 0.063(3) Uani 1 d . .
H26A H 1.0272(11) 0.3736(7) 0.2046(7) 0.075 Uiso 1 calc R .
C27 C 1.4095(11) 0.3516(8) 0.1391(8) 0.083(4) Uani 1 d . .
H27A H 1.4063(11) 0.4026(8) 0.1384(8) 0.124 Uiso 1 calc R .
H27B H 1.4167(11) 0.3343(8) 0.0881(8) 0.124 Uiso 1 calc R .
H27C H 1.4799(11) 0.3362(8) 0.1759(8) 0.124 Uiso 1 calc R .
C28 C 0.7151(12) 0.3429(7) 0.3524(7) 0.071(4) Uani 1 d . .
H28A H 0.8017(12) 0.3496(7) 0.3746(7) 0.086 Uiso 1 calc R .
H28B H 0.6697(12) 0.3349(7) 0.3949(7) 0.086 Uiso 1 calc R .
C29 C 0.6672(12) 0.4091(7) 0.3094(7) 0.063(3) Uani 1 d . .
C30 C 0.7332(14) 0.4389(8) 0.2570(9) 0.080(4) Uani 1 d . .
H30A H 0.8065(14) 0.4178(8) 0.2481(9) 0.096 Uiso 1 calc R .
C31 C 0.6916(19) 0.4992(9) 0.2181(10) 0.110(6) Uani 1 d . .
H31A H 0.7361(19) 0.5186(9) 0.1820(10) 0.132 Uiso 1 calc R .
C32 C 0.5862(22) 0.5317(9) 0.2310(12) 0.133(8) Uani 1 d . .
H32A H 0.5594(22) 0.5735(9) 0.2050(12) 0.160 Uiso 1 calc R .
C33 C 0.5213(20) 0.5023(11) 0.2819(11) 0.131(7) Uani 1 d . .
H33A H 0.4470(20) 0.5231(11) 0.2893(11) 0.157 Uiso 1 calc R .
C34 C 0.5626(16) 0.4419(9) 0.3234(9) 0.099(5) Uani 1 d . .
H34A H 0.5191(16) 0.4237(9) 0.3606(9) 0.119 Uiso 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'
I I -0.4742 1.8119 '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
N8 Re N4 85.7(3) . . y
N8 Re N5 75.6(3) . . y
N4 Re N5 109.7(3) . . y
N8 Re N1 106.8(3) . . y
N4 Re N1 74.4(3) . . y
N5 Re N1 175.5(3) . . y
N8 Re I1 93.8(2) . . y
N4 Re I1 161.8(2) . . y
N5 Re I1 87.6(2) . . y
N1 Re I1 88.4(2) . . y
N8 Re I2 160.6(2) . . y
N4 Re I2 90.4(2) . . y
N5 Re I2 88.0(3) . . y
N1 Re I2 90.3(2) . . y
I1 Re I2 95.75(4) . . y
C3 N1 C1 106.4(8) . . ?
C3 N1 Re 112.7(7) . . ?
C1 N1 Re 140.8(7) . . ?
C3 N2 C2 106.0(9) . . ?
C3 N2 C11 126.2(10) . . ?
C2 N2 C11 127.7(10) . . ?
C3 N3 N4 108.0(8) . . ?
N3 N4 C4 112.0(8) . . ?
N3 N4 Re 121.6(6) . . ?
C4 N4 Re 125.8(6) . . ?
C20 N5 C19 105.9(9) . . ?
C20 N5 Re 112.0(6) . . ?
C19 N5 Re 141.3(8) . . ?
C20 N6 C18 106.1(10) . . ?
C20 N6 C28 126.3(10) . . ?
C18 N6 C28 126.9(10) . . ?
C20 N7 N8 108.6(9) . . ?
N7 N8 C21 112.8(9) . . ?
N7 N8 Re 121.0(7) . . ?
C21 N8 Re 125.6(7) . . ?
N1 C1 C2 107.2(10) . . ?
N2 C2 C1 109.5(10) . . ?
N3 C3 N1 122.8(9) . . ?
N3 C3 N2 126.3(10) . . ?
N1 C3 N2 110.9(10) . . ?
C9 C4 C5 120.7(10) . . ?
C9 C4 N4 121.0(9) . . ?
C5 C4 N4 118.2(9) . . ?
C4 C5 C6 118.3(11) . . ?
C7 C6 C5 121.2(12) . . ?
C6 C7 C8 119.7(12) . . ?
C6 C7 C10 121.3(13) . . ?
C8 C7 C10 118.6(14) . . ?
C7 C8 C9 119.9(12) . . ?
C4 C9 C8 120.0(11) . . ?
N2 C11 C12 112.9(9) . . ?
C13 C12 C17 120.2(12) . . ?
C13 C12 C11 120.0(11) . . ?
C17 C12 C11 119.7(12) . . ?
C12 C13 C14 119.1(13) . . ?
C15 C14 C13 121.9(15) . . ?
C16 C15 C14 119.8(15) . . ?
C15 C16 C17 119.7(14) . . ?
C16 C17 C12 119.3(14) . . ?
C19 C18 N6 109.2(10) . . ?
C18 C19 N5 108.5(11) . . ?
N7 C20 N5 122.3(9) . . ?
N7 C20 N6 127.4(11) . . ?
N5 C20 N6 110.3(9) . . ?
C22 C21 C26 119.9(11) . . ?
C22 C21 N8 119.3(10) . . ?
C26 C21 N8 120.7(10) . . ?
C21 C22 C23 119.7(12) . . ?
C24 C23 C22 121.9(12) . . ?
C23 C24 C25 118.0(12) . . ?
C23 C24 C27 121.2(12) . . ?
C25 C24 C27 120.8(12) . . ?
C26 C25 C24 121.4(12) . . ?
C25 C26 C21 118.9(11) . . ?
N6 C28 C29 112.4(10) . . ?
C34 C29 C30 119.2(14) . . ?
C34 C29 C28 121.4(13) . . ?
C30 C29 C28 119.3(12) . . ?
C31 C30 C29 120.0(14) . . ?
C30 C31 C32 121.1(17) . . ?
C33 C32 C31 118.9(19) . . ?
C32 C33 C34 121.3(18) . . ?
C29 C34 C33 119.4(16) . . ?
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 N8 2.000(9) . y
Re N4 2.041(8) . y
Re N5 2.053(8) . y
Re N1 2.065(8) . y
Re I1 2.7214(10) . y
Re I2 2.7412(12) . y
N1 C3 1.338(12) . ?
N1 C1 1.362(12) . ?
N2 C3 1.347(12) . ?
N2 C2 1.337(14) . ?
N2 C11 1.463(13) . ?
N3 C3 1.341(12) . ?
N3 N4 1.339(10) . y
N4 C4 1.433(12) . ?
N5 C20 1.358(13) . ?
N5 C19 1.375(12) . ?
N6 C20 1.361(12) . ?
N6 C18 1.360(15) . ?
N6 C28 1.452(13) . ?
N7 C20 1.315(13) . ?
N7 N8 1.366(11) . y
N8 C21 1.420(13) . ?
C1 C2 1.361(15) . ?
C4 C9 1.351(13) . ?
C4 C5 1.383(14) . ?
C5 C6 1.40(2) . ?
C6 C7 1.35(2) . ?
C7 C8 1.38(2) . ?
C7 C10 1.54(2) . ?
C8 C9 1.390(15) . ?
C11 C12 1.501(15) . ?
C12 C13 1.37(2) . ?
C12 C17 1.39(2) . ?
C13 C14 1.37(2) . ?
C14 C15 1.37(2) . ?
C15 C16 1.36(2) . ?
C16 C17 1.41(2) . ?
C18 C19 1.346(15) . ?
C21 C22 1.377(15) . ?
C21 C26 1.38(2) . ?
C22 C23 1.37(2) . ?
C23 C24 1.35(2) . ?
C24 C25 1.39(2) . ?
C24 C27 1.51(2) . ?
C25 C26 1.37(2) . ?
C28 C29 1.50(2) . ?
C29 C34 1.36(2) . ?
C29 C30 1.37(2) . ?
C30 C31 1.36(2) . ?
C31 C32 1.36(2) . ?
C32 C33 1.34(2) . ?
C33 C34 1.38(2) . ?
