#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/91/4319158.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_4319158
loop_
_publ_author_name
'Sibaprasad Bhattacharyya'
'Indranil Chakraborty'
'Bimal Kumar Dirghangi'
'Animesh Chakravorty'
_publ_section_title
;
 Oxygen Atom Transfer from Nitrogenous ReVO Reagents to Diphosphines and
 Subsequent Transformations. Rhenium(III) Products and Reaction Models
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              286
_journal_page_last               293
_journal_paper_doi               10.1021/ic0005893
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        'laboratory synthesis'
_chemical_formula_sum            'C36 H30 Cl4 N3 O2 P2 Re'
_chemical_formula_weight         926.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 99.22(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.866(6)
_cell_length_b                   12.583(6)
_cell_length_c                   34.778(23)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      7
_cell_volume                     7285(7)
_computing_cell_refinement       'Siemens P3/P4 V-4.27'
_computing_data_collection       'Siemens P3/P4 V-4.27'
_computing_data_reduction        'Siemens P3/P4 V-4.27'
_computing_molecular_graphics    'Siemens SHELXTL V-5.03 PC'
_computing_publication_material  'Siemens SHELXTL V-5.03 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  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0721
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            6073
_diffrn_reflns_theta_max         24.05
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.754
_exptl_absorpt_correction_T_max  0.2217
_exptl_absorpt_correction_T_min  0.1486
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            Dark
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_description       Parallelopiped
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.863
_refine_diff_density_min         -1.592
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.023
_refine_ls_goodness_of_fit_obs   1.007
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_restrained_S_obs      1.007
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_obs          0.0571
_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)+(0.0000P)²+241.0809P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1375
_refine_ls_wR_factor_obs         0.1019
_reflns_number_observed          3556
_reflns_number_total             5704
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0005893_4.cif
_cod_data_source_block           625re1
_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^)+(0.0000P)^2^+241.0809P] 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^)+(0.0000P)^2^+241.0809P] 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        7285.4(65)
_cod_database_code               4319158
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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 0.12043(4) 0.78628(4) 0.082417(15) 0.0523(2) Uani 1 d . .
Cl1 Cl 0.0679(3) 0.9108(3) 0.12338(12) 0.0835(13) Uani 1 d . .
Cl2 Cl 0.2505(2) 0.8315(3) 0.11369(10) 0.0756(11) Uani 1 d . .
Cl3 Cl -0.0127(2) 0.7369(3) 0.05618(10) 0.0690(10) Uani 1 d . .
P1 P 0.0737(2) 0.6008(3) 0.14652(9) 0.0481(9) Uani 1 d . .
P2 P -0.0776(2) 0.6359(3) 0.18810(9) 0.0486(9) Uani 1 d . .
N1 N 0.1233(7) 0.8896(9) 0.0380(3) 0.061(3) Uani 1 d . .
N2 N 0.1580(7) 0.7369(9) 0.0059(3) 0.059(3) Uani 1 d . .
N3 N 0.1580(6) 0.7014(9) 0.0414(3) 0.054(3) Uani 1 d . .
O1 O 0.1219(5) 0.6665(6) 0.1216(2) 0.054(2) Uani 1 d . .
O2 O -0.1033(6) 0.5246(7) 0.1826(3) 0.066(3) Uani 1 d . .
C1 C 0.1414(9) 0.8430(12) 0.0044(4) 0.059(4) Uani 1 d . .
C2 C 0.1414(10) 0.9020(13) -0.0297(4) 0.077(5) Uani 1 d . .
H2A H 0.1510(10) 0.8688(13) -0.0524(4) 0.092 Uiso 1 calc R .
C3 C 0.1274(10) 1.0065(15) -0.0294(4) 0.082(5) Uani 1 d . .
H3A H 0.1294(10) 1.0468(15) -0.0516(4) 0.098 Uiso 1 calc R .
C4 C 0.1100(11) 1.0550(13) 0.0043(5) 0.098(6) Uani 1 d . .
H4A H 0.0982(11) 1.1272(13) 0.0042(5) 0.118 Uiso 1 calc R .
C5 C 0.1100(10) 0.9969(11) 0.0371(5) 0.077(5) Uani 1 d . .
H5A H 0.1008(10) 1.0310(11) 0.0596(5) 0.092 Uiso 1 calc R .
C6 C 0.1774(8) 0.5905(11) 0.0456(3) 0.054(4) Uani 1 d . .
C7 C 0.2353(8) 0.5578(12) 0.0766(4) 0.058(4) Uani 1 d . .
H7A H 0.2598(8) 0.6064(12) 0.0949(4) 0.070 Uiso 1 calc R .
C8 C 0.2551(8) 0.4517(13) 0.0794(4) 0.064(4) Uani 1 d . .
H8A H 0.2919(8) 0.4277(13) 0.1004(4) 0.077 Uiso 1 calc R .
C9 C 0.2215(10) 0.3814(12) 0.0519(4) 0.074(5) Uani 1 d . .
C10 C 0.1631(11) 0.4123(12) 0.0221(4) 0.079(5) Uani 1 d . .
H10A H 0.1380(11) 0.3622(12) 0.0046(4) 0.095 Uiso 1 calc R .
C11 C 0.1417(9) 0.5173(12) 0.0181(4) 0.069(4) Uani 1 d . .
H11A H 0.1037(9) 0.5395(12) -0.0028(4) 0.083 Uiso 1 calc R .
C12 C 0.0410(8) 0.4779(11) 0.1234(3) 0.052(3) Uani 1 d . .
C13 C -0.0334(10) 0.4670(13) 0.1014(4) 0.075(5) Uani 1 d . .
H13A H -0.0699(10) 0.5229(13) 0.1000(4) 0.090 Uiso 1 calc R .
C14 C -0.0551(9) 0.3740(14) 0.0814(4) 0.076(5) Uani 1 d . .
H14A H -0.1057(9) 0.3671(14) 0.0664(4) 0.091 Uiso 1 calc R .
C15 C -0.0006(9) 0.2919(12) 0.0839(4) 0.065(4) Uani 1 d . .
H15A H -0.0143(9) 0.2282(12) 0.0710(4) 0.078 Uiso 1 calc R .
C16 C 0.0734(9) 0.3046(13) 0.1054(4) 0.082(5) Uani 1 d . .
H16A H 0.1107(9) 0.2498(13) 0.1061(4) 0.098 Uiso 1 calc R .
C17 C 0.0947(9) 0.3958(11) 0.1260(4) 0.061(4) Uani 1 d . .
H17A H 0.1449(9) 0.4019(11) 0.1414(4) 0.074 Uiso 1 calc R .
C18 C 0.1365(8) 0.5740(10) 0.1913(3) 0.044(3) Uani 1 d . .
C19 C 0.2084(9) 0.6336(12) 0.2000(4) 0.069(4) Uani 1 d . .
H19A H 0.2238(9) 0.6800(12) 0.1817(4) 0.083 Uiso 1 calc R .
C20 C 0.2551(10) 0.6216(12) 0.2361(4) 0.077(5) Uani 1 d . .
H20A H 0.3019(10) 0.6614(12) 0.2424(4) 0.092 Uiso 1 calc R .
C21 C 0.2336(9) 0.5521(13) 0.2625(4) 0.072(4) Uani 1 d . .
H21A H 0.2658(9) 0.5445(13) 0.2867(4) 0.087 Uiso 1 calc R .
C22 C 0.1643(9) 0.4929(11) 0.2538(4) 0.066(4) Uani 1 d . .
H22A H 0.1494(9) 0.4464(11) 0.2721(4) 0.079 Uiso 1 calc R .
C23 C 0.1167(8) 0.5028(11) 0.2176(3) 0.055(4) Uani 1 d . .
H23A H 0.0712(8) 0.4606(11) 0.2112(3) 0.066 Uiso 1 calc R .
C24 C -0.0094(8) 0.6776(10) 0.1552(3) 0.054(3) Uani 1 d . .
H24A H -0.0423(8) 0.6896(10) 0.1300(3) 0.064 Uiso 1 calc R .
H24B H 0.0117(8) 0.7463(10) 0.1644(3) 0.064 Uiso 1 calc R .
C25 C -0.1591(7) 0.7284(10) 0.1791(3) 0.049(3) Uani 1 d . .
C26 C -0.1613(9) 0.8193(11) 0.1555(4) 0.068(4) Uani 1 d . .
H26A H -0.1177(9) 0.8360(11) 0.1433(4) 0.082 Uiso 1 calc R .
C27 C -0.2299(11) 0.8851(12) 0.1502(4) 0.079(5) Uani 1 d . .
H27A H -0.2324(11) 0.9446(12) 0.1343(4) 0.095 Uiso 1 calc R .
C28 C -0.2915(11) 0.8601(15) 0.1687(5) 0.087(6) Uani 1 d . .
H28A H -0.3362(11) 0.9044(15) 0.1658(5) 0.105 Uiso 1 calc R .
C29 C -0.2909(9) 0.7740(15) 0.1912(5) 0.089(5) Uani 1 d . .
H29A H -0.3351(9) 0.7589(15) 0.2032(5) 0.106 Uiso 1 calc R .
C30 C -0.2254(9) 0.7078(12) 0.1968(4) 0.069(4) Uani 1 d . .
H30A H -0.2256(9) 0.6483(12) 0.2127(4) 0.083 Uiso 1 calc R .
C31 C -0.0288(8) 0.6644(10) 0.2373(3) 0.048(3) Uani 1 d . .
C32 C 0.0081(9) 0.7583(11) 0.2487(4) 0.063(4) Uani 1 d . .
H32A H 0.0097(9) 0.8120(11) 0.2304(4) 0.076 Uiso 1 calc R .
C33 C 0.0428(9) 0.7746(14) 0.2867(4) 0.082(5) Uani 1 d . .
H33A H 0.0683(9) 0.8386(14) 0.2940(4) 0.099 Uiso 1 calc R .
C34 C 0.0399(10) 0.6976(16) 0.3136(4) 0.085(5) Uani 1 d . .
H34A H 0.0637(10) 0.7091(16) 0.3393(4) 0.102 Uiso 1 calc R .
C35 C 0.0021(10) 0.6020(14) 0.3033(4) 0.075(5) Uani 1 d . .
H35A H 0.0004(10) 0.5494(14) 0.3220(4) 0.090 Uiso 1 calc R .
C36 C -0.0333(9) 0.5855(11) 0.2651(4) 0.062(4) Uani 1 d . .
H36A H -0.0600(9) 0.5221(11) 0.2579(4) 0.075 Uiso 1 calc R .
Cl4 Cl 0.2482(3) 0.2472(3) 0.05552(15) 0.111(2) 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'
O O 0.0106 0.0060 '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
N3 Re N1 75.3(5) . . y
N3 Re O1 96.5(4) . . y
N1 Re O1 171.8(4) . . y
N3 Re Cl2 94.7(3) . . y
N1 Re Cl2 93.6(3) . . y
O1 Re Cl2 87.7(3) . . y
N3 Re Cl3 88.5(3) . . y
N1 Re Cl3 90.6(3) . . y
O1 Re Cl3 88.4(3) . . y
Cl2 Re Cl3 175.21(12) . . y
N3 Re Cl1 170.1(3) . . y
N1 Re Cl1 95.2(4) . . y
O1 Re Cl1 93.0(2) . . y
Cl2 Re Cl1 88.5(2) . . y
Cl3 Re Cl1 89.0(2) . . y
O1 P1 C24 108.0(5) . . ?
O1 P1 C18 107.8(5) . . ?
C24 P1 C18 109.4(5) . . ?
O1 P1 C12 111.6(5) . . ?
C24 P1 C12 110.7(6) . . ?
C18 P1 C12 109.2(6) . . ?
O2 P2 C25 113.3(6) . . ?
O2 P2 C31 113.1(6) . . ?
C25 P2 C31 104.9(5) . . ?
O2 P2 C24 113.2(6) . . ?
C25 P2 C24 104.3(6) . . ?
C31 P2 C24 107.4(6) . . ?
C5 N1 C1 117.0(12) . . ?
C5 N1 Re 128.9(10) . . ?
C1 N1 Re 114.1(9) . . ?
N3 N2 C1 109.7(11) . . ?
N2 N3 C6 113.0(11) . . ?
N2 N3 Re 123.1(9) . . y
C6 N3 Re 123.4(8) . . ?
P1 O1 Re 146.7(5) . . y
N2 C1 N1 117.0(11) . . ?
N2 C1 C2 121.6(14) . . ?
N1 C1 C2 121.4(14) . . ?
C3 C2 C1 119.5(15) . . ?
C2 C3 C4 119.9(15) . . ?
C5 C4 C3 119.9(16) . . ?
C4 C5 N1 122.1(16) . . ?
C11 C6 C7 120.5(13) . . ?
C11 C6 N3 120.4(12) . . ?
C7 C6 N3 119.0(13) . . ?
C8 C7 C6 118.2(14) . . ?
C9 C8 C7 120.9(14) . . ?
C8 C9 C10 121.2(14) . . ?
C8 C9 Cl4 120.3(13) . . ?
C10 C9 Cl4 118.4(13) . . ?
C9 C10 C11 119.8(15) . . ?
C10 C11 C6 119.3(14) . . ?
C17 C12 C13 120.0(13) . . ?
C17 C12 P1 118.0(10) . . ?
C13 C12 P1 121.8(11) . . ?
C12 C13 C14 120.8(15) . . ?
C15 C14 C13 118.9(14) . . ?
C16 C15 C14 119.5(14) . . ?
C15 C16 C17 121.8(14) . . ?
C12 C17 C16 118.9(13) . . ?
C23 C18 C19 120.1(12) . . ?
C23 C18 P1 122.7(11) . . ?
C19 C18 P1 117.2(9) . . ?
C20 C19 C18 118.7(14) . . ?
C21 C20 C19 120.7(15) . . ?
C20 C21 C22 120.4(13) . . ?
C21 C22 C23 120.0(13) . . ?
C18 C23 C22 120.1(14) . . ?
P1 C24 P2 123.2(7) . . y
C30 C25 C26 117.7(13) . . ?
C30 C25 P2 116.9(11) . . ?
C26 C25 P2 125.5(11) . . ?
C25 C26 C27 119.9(15) . . ?
C28 C27 C26 118.8(16) . . ?
C29 C28 C27 122.4(17) . . ?
C28 C29 C30 120.4(17) . . ?
C29 C30 C25 120.7(16) . . ?
C32 C31 C36 119.2(12) . . ?
C32 C31 P2 124.2(10) . . ?
C36 C31 P2 116.5(11) . . ?
C31 C32 C33 120.8(14) . . ?
C34 C33 C32 120.1(16) . . ?
C33 C34 C35 120.8(15) . . ?
C34 C35 C36 119.3(14) . . ?
C35 C36 C31 119.7(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 1.966(11) . y
Re N1 2.026(10) . y
Re O1 2.030(7) . y
Re Cl2 2.357(4) . y
Re Cl3 2.368(4) . y
Re Cl1 2.382(4) . y
P1 O1 1.523(8) . y
P1 C24 1.769(12) . ?
P1 C18 1.771(12) . ?
P1 C12 1.789(13) . ?
P2 O2 1.469(9) . y
P2 C25 1.789(13) . ?
P2 C31 1.812(12) . ?
P2 C24 1.824(12) . ?
N1 C5 1.37(2) . ?
N1 C1 1.38(2) . ?
N2 N3 1.316(13) . y
N2 C1 1.36(2) . ?
N3 C6 1.43(2) . ?
C1 C2 1.40(2) . ?
C2 C3 1.34(2) . ?
C3 C4 1.39(2) . ?
C4 C5 1.35(2) . ?
C6 C11 1.39(2) . ?
C6 C7 1.40(2) . ?
C7 C8 1.38(2) . ?
C8 C9 1.36(2) . ?
C9 C10 1.37(2) . ?
C9 Cl4 1.747(15) . ?
C10 C11 1.37(2) . ?
C12 C17 1.37(2) . ?
C12 C13 1.37(2) . ?
C13 C14 1.38(2) . ?
C14 C15 1.38(2) . ?
C15 C16 1.36(2) . ?
C16 C17 1.37(2) . ?
C18 C23 1.36(2) . ?
C18 C19 1.42(2) . ?
C19 C20 1.38(2) . ?
C20 C21 1.36(2) . ?
C21 C22 1.38(2) . ?
C22 C23 1.39(2) . ?
C25 C30 1.39(2) . ?
C25 C26 1.40(2) . ?
C26 C27 1.41(2) . ?
C27 C28 1.34(2) . ?
C28 C29 1.34(2) . ?
C29 C30 1.37(2) . ?
C31 C32 1.36(2) . ?
C31 C36 1.40(2) . ?
C32 C33 1.37(2) . ?
C33 C34 1.35(2) . ?
C34 C35 1.38(2) . ?
C35 C36 1.38(2) . ?
