#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/79/4317927.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_4317927
loop_
_publ_author_name
'Jaydip Gangopadhyay'
'Suman Sengupta'
'Sibaprasad Bhattacharyya'
'Indranil Chakraborty'
'Animesh Chakravorty'
_publ_section_title
;
 Pyridylazole Chelation of Oxorhenium(V) and Imidorhenium(V). Rates and
 Trends of Oxygen Atom Transfer from ReVO to Tertiary Phosphines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2616
_journal_page_last               2622
_journal_paper_doi               10.1021/ic011064t
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C18 H13 Cl3 N3 O Re'
_chemical_formula_weight         579.86
_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                 94.03(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.566(6)
_cell_length_b                   16.082(8)
_cell_length_c                   11.841(5)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7
_cell_volume                     1817.1(16)
_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  0.1007
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3371
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    7.141
_exptl_absorpt_correction_T_max  0.277
_exptl_absorpt_correction_T_min  0.152
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            dark_blue
_exptl_crystal_density_diffrn    2.120
_exptl_crystal_description       parallelopiped
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         4.861
_refine_diff_density_min         -3.944
_refine_diff_density_rms         0.326
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.238
_refine_ls_goodness_of_fit_obs   1.288
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3164
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.356
_refine_ls_restrained_S_obs      1.288
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_obs          0.0582
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1793
_refine_ls_wR_factor_obs         0.1510
_reflns_number_observed          2497
_reflns_number_total             3182
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic011064t_4.cif
_cod_data_source_block           nar[Re(NPh)Cl3(pbo)]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^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^)+(0.1000P)^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 

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        1817.0(16)
_cod_database_code               4317927
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 0.69648(5) 0.85206(3) 0.24440(4) 0.0224(2) Uani 1 d . .
Cl3 Cl 0.5033(3) 0.7906(2) 0.1479(3) 0.0365(7) Uani 1 d . .
Cl2 Cl 0.8383(3) 0.9414(2) 0.3625(3) 0.0364(7) Uani 1 d . .
Cl1 Cl 0.6401(4) 0.7805(2) 0.4055(3) 0.0376(8) Uani 1 d . .
O O 0.6396(9) 1.0656(5) 0.0502(8) 0.034(2) Uani 1 d . .
N1 N 0.5359(10) 0.9494(6) 0.2845(8) 0.025(2) Uani 1 d . .
N2 N 0.7002(10) 0.9420(6) 0.1189(9) 0.028(2) Uani 1 d . .
N3 N 0.8306(10) 0.7921(6) 0.2049(9) 0.025(2) Uiso 1 d . .
C1 C 0.4522(13) 0.9464(8) 0.3694(10) 0.032(3) Uani 1 d . .
H1A H 0.4507(13) 0.8996(8) 0.4153(10) 0.039 Uiso 1 calc R .
C2 C 0.3656(15) 1.0152(10) 0.3889(13) 0.049(4) Uani 1 d . .
H2A H 0.3059(15) 1.0134(10) 0.4475(13) 0.058 Uiso 1 calc R .
C3 C 0.3689(15) 1.0830(9) 0.3236(14) 0.047(4) Uani 1 d . .
H3A H 0.3145(15) 1.1290(9) 0.3390(14) 0.056 Uiso 1 calc R .
C4 C 0.4518(13) 1.0847(8) 0.2344(12) 0.034(3) Uani 1 d . .
H4A H 0.4524(13) 1.1302(8) 0.1861(12) 0.041 Uiso 1 calc R .
C5 C 0.5337(12) 1.0168(7) 0.2191(10) 0.025(2) Uiso 1 d . .
C6 C 0.6269(12) 1.0069(7) 0.1278(10) 0.025(2) Uiso 1 d . .
C7 C 0.7741(12) 0.9543(7) 0.0228(9) 0.023(2) Uani 1 d . .
C8 C 0.8659(13) 0.9077(8) -0.0300(11) 0.032(3) Uani 1 d . .
H8A H 0.8925(13) 0.8550(8) -0.0044(11) 0.038 Uiso 1 calc R .
C9 C 0.9189(14) 0.9431(8) -0.1255(11) 0.038(3) Uani 1 d . .
H9A H 0.9804(14) 0.9123(8) -0.1663(11) 0.045 Uiso 1 calc R .
C10 C 0.8836(14) 1.0219(9) -0.1613(12) 0.042(3) Uani 1 d . .
H10A H 0.9261(14) 1.0442(9) -0.2227(12) 0.050 Uiso 1 calc R .
C11 C 0.7880(14) 1.0682(9) -0.1093(12) 0.041(3) Uani 1 d . .
H11A H 0.7610(14) 1.1207(9) -0.1356(12) 0.050 Uiso 1 calc R .
C12 C 0.7344(13) 1.0338(7) -0.0173(10) 0.029(3) Uani 1 d . .
C13 C 0.9537(12) 0.7511(7) 0.1902(10) 0.026(3) Uani 1 d . .
C14 C 1.0649(15) 0.7609(7) 0.2696(12) 0.037(3) Uani 1 d . .
H14A H 1.0569(15) 0.7956(7) 0.3317(12) 0.044 Uiso 1 calc R .
C15 C 1.1859(13) 0.7197(9) 0.2563(13) 0.045(4) Uani 1 d . .
H15A H 1.2624(13) 0.7269(9) 0.3083(13) 0.054 Uiso 1 calc R .
C16 C 1.1952(16) 0.6684(9) 0.1681(17) 0.056(5) Uani 1 d . .
H16A H 1.2786(16) 0.6400(9) 0.1600(17) 0.067 Uiso 1 calc R .
C17 C 1.0846(18) 0.6566(8) 0.0892(16) 0.052(4) Uani 1 d . .
H17A H 1.0920(18) 0.6202(8) 0.0290(16) 0.062 Uiso 1 calc R .
C18 C 0.9646(13) 0.6993(7) 0.1014(11) 0.032(3) Uani 1 d . .
H18A H 0.8891(13) 0.6930(7) 0.0482(11) 0.039 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'
O O 0.0106 0.0060 '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
N3 Re N2 98.5(4) . . y
N3 Re N1 170.7(4) . . y
N2 Re N1 73.4(3) . . y
N3 Re Cl1 99.7(3) . . y
N2 Re Cl1 161.7(3) . . y
N1 Re Cl1 88.3(2) . . y
N3 Re Cl3 102.3(3) . . y
N2 Re Cl3 89.9(3) . . y
N1 Re Cl3 82.5(3) . . y
Cl1 Re Cl3 88.32(13) . . y
N3 Re Cl2 95.4(4) . . y
N2 Re Cl2 87.8(3) . . y
N1 Re Cl2 80.0(3) . . y
Cl1 Re Cl2 88.39(12) . . y
Cl3 Re Cl2 162.25(11) . . y
C6 O C12 103.8(9) . . ?
C1 N1 C5 118.9(10) . . ?
C1 N1 Re 125.9(8) . . ?
C5 N1 Re 115.1(7) . . ?
C6 N2 C7 105.4(10) . . ?
C6 N2 Re 118.5(8) . . ?
C7 N2 Re 135.9(8) . . ?
C13 N3 Re 168.8(9) . . ?
N1 C1 C2 119.2(13) . . ?
C3 C2 C1 120.4(13) . . ?
C2 C3 C4 120.1(13) . . ?
C3 C4 C5 117.2(13) . . ?
N1 C5 C4 124.1(11) . . ?
N1 C5 C6 111.0(9) . . ?
C4 C5 C6 124.9(11) . . ?
N2 C6 O 116.7(10) . . ?
N2 C6 C5 121.5(10) . . ?
O C6 C5 121.8(10) . . ?
C8 C7 N2 133.3(11) . . ?
C8 C7 C12 121.4(10) . . ?
N2 C7 C12 105.3(10) . . ?
C7 C8 C9 115.9(12) . . ?
C10 C9 C8 122.2(12) . . ?
C11 C10 C9 121.7(12) . . ?
C12 C11 C10 116.4(13) . . ?
O C12 C11 129.0(12) . . ?
O C12 C7 108.7(9) . . ?
C11 C12 C7 122.3(12) . . ?
C18 C13 N3 120.6(11) . . ?
C18 C13 C14 120.3(11) . . ?
N3 C13 C14 119.1(11) . . ?
C15 C14 C13 119.3(12) . . ?
C16 C15 C14 119.9(13) . . ?
C15 C16 C17 121.6(13) . . ?
C18 C17 C16 118.4(14) . . ?
C13 C18 C17 120.5(14) . . ?
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 N3 1.698(9) . y
Re N2 2.077(10) . y
Re N1 2.267(9) . y
Re Cl1 2.324(3) . y
Re Cl3 2.324(3) . y
Re Cl2 2.365(3) . y
O C6 1.328(14) . ?
O C12 1.350(14) . ?
N1 C1 1.330(15) . ?
N1 C5 1.331(14) . ?
N2 C6 1.266(14) . ?
N2 C7 1.395(14) . ?
N3 C13 1.371(14) . ?
C1 C2 1.41(2) . ?
C2 C3 1.34(2) . ?
C3 C4 1.36(2) . ?
C4 C5 1.36(2) . ?
C5 C6 1.46(2) . ?
C7 C8 1.34(2) . ?
C7 C12 1.41(2) . ?
C8 C9 1.39(2) . ?
C9 C10 1.37(2) . ?
C10 C11 1.36(2) . ?
C11 C12 1.36(2) . ?
C13 C18 1.35(2) . ?
C13 C14 1.38(2) . ?
C14 C15 1.35(2) . ?
C15 C16 1.34(2) . ?
C16 C17 1.37(2) . ?
C17 C18 1.35(2) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30661057
