#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:57:53 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179271 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/91/4319156.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_4319156
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        'laboratoy synthesis'
_chemical_formula_sum            'C30 H25 Cl6 N3 P Re'
_chemical_formula_weight         857.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'Patterson heavy atom'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 100.94(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.695(6)
_cell_length_b                   17.745(7)
_cell_length_c                   15.459(9)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      7
_cell_volume                     3150(3)
_computing_cell_refinement       'Siemens P3/P4 V-4.27 PC'
_computing_data_collection       'Siemens P3/P4 V-4.27 PC'
_computing_data_reduction        'Siemens P3/P4 V-4.27 PC'
_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 scan'
_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  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6002
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.444
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.325
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_description       Parallelopiped
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.494
_refine_diff_density_min         -4.607
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.040
_refine_ls_goodness_of_fit_obs   1.063
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_restrained_S_obs      1.063
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_obs          0.0585
_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)+(0.0896P)²+18.3209P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1656
_refine_ls_wR_factor_obs         0.1403
_reflns_number_observed          4032
_reflns_number_total             5564
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0005893_2.cif
_cod_data_source_block           616re
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0896P)^2^+18.3209P] 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^)+(0.0896P)^2^+18.3209P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3149.9(27)
_cod_database_code               4319156
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.39734(4) 0.88937(2) 0.15661(3) 0.0349(2) Uani 1 d . .
Cl1 Cl 0.5241(3) 0.8641(2) 0.0569(2) 0.0594(8) Uani 1 d . .
Cl2 Cl 0.3289(3) 0.9981(2) 0.0792(2) 0.0477(7) Uani 1 d . .
Cl3 Cl 0.2563(3) 0.8113(2) 0.0691(2) 0.0564(8) Uani 1 d . .
Cl4 Cl 0.6814(4) 1.2489(2) 0.2886(3) 0.0869(13) Uani 1 d . .
Cl5 Cl 0.5669(6) 0.5852(4) 0.0736(5) 0.149(3) Uani 1 d . .
Cl6 Cl 0.4248(5) 0.6632(4) -0.0706(3) 0.116(2) Uani 1 d . .
P1 P 0.2524(3) 0.9138(2) 0.2541(2) 0.0358(6) Uani 1 d . .
N1 N 0.4671(8) 0.7983(5) 0.2332(5) 0.039(2) Uani 1 d . .
N2 N 0.6015(9) 0.8867(6) 0.3003(6) 0.049(2) Uani 1 d . .
N3 N 0.5330(8) 0.9300(6) 0.2418(6) 0.047(2) Uani 1 d . .
C1 C 0.5644(10) 0.8133(6) 0.2939(7) 0.043(3) Uani 1 d . .
C2 C 0.6222(11) 0.7589(8) 0.3495(8) 0.057(3) Uani 1 d . .
H2A H 0.6892(11) 0.7714(8) 0.3897(8) 0.068 Uiso 1 calc R .
C3 C 0.5808(12) 0.6869(8) 0.3452(9) 0.062(4) Uani 1 d . .
H3A H 0.6190(12) 0.6497(8) 0.3821(9) 0.075 Uiso 1 calc R .
C4 C 0.4787(13) 0.6703(7) 0.2835(9) 0.061(3) Uani 1 d . .
H4A H 0.4483(13) 0.6217(7) 0.2787(9) 0.073 Uiso 1 calc R .
C5 C 0.4252(11) 0.7268(6) 0.2309(7) 0.048(3) Uani 1 d . .
H5A H 0.3566(11) 0.7158(6) 0.1917(7) 0.057 Uiso 1 calc R .
C6 C 0.5715(9) 1.0087(6) 0.2513(7) 0.038(2) Uani 1 d . .
C7 C 0.5867(9) 1.0491(6) 0.1781(7) 0.040(2) Uani 1 d . .
H7A H 0.5739(9) 1.0266(6) 0.1227(7) 0.048 Uiso 1 calc R .
C8 C 0.6220(10) 1.1246(7) 0.1886(9) 0.053(3) Uani 1 d . .
H8A H 0.6312(10) 1.1538(7) 0.1404(9) 0.063 Uiso 1 calc R .
C9 C 0.6426(11) 1.1546(7) 0.2731(9) 0.055(3) Uani 1 d . .
C10 C 0.6304(13) 1.1129(7) 0.3460(8) 0.061(4) Uani 1 d . .
H10A H 0.6468(13) 1.1342(7) 0.4019(8) 0.073 Uiso 1 calc R .
C11 C 0.5934(11) 1.0394(7) 0.3346(8) 0.053(3) Uani 1 d . .
H11A H 0.5834(11) 1.0105(7) 0.3829(8) 0.064 Uiso 1 calc R .
C12 C 0.2514(10) 0.8346(6) 0.3283(7) 0.039(2) Uani 1 d . .
C13 C 0.1616(10) 0.7830(7) 0.3176(8) 0.050(3) Uani 1 d . .
H13A H 0.0969(10) 0.7906(7) 0.2732(8) 0.060 Uiso 1 calc R .
C14 C 0.1656(14) 0.7203(8) 0.3713(10) 0.069(4) Uani 1 d . .
H14A H 0.1053(14) 0.6854(8) 0.3612(10) 0.083 Uiso 1 calc R .
C15 C 0.2581(13) 0.7095(7) 0.4393(8) 0.057(3) Uani 1 d . .
H15A H 0.2592(13) 0.6684(7) 0.4768(8) 0.069 Uiso 1 calc R .
C16 C 0.3484(12) 0.7595(7) 0.4516(8) 0.056(3) Uani 1 d . .
H16A H 0.4123(12) 0.7515(7) 0.4966(8) 0.067 Uiso 1 calc R .
C17 C 0.3456(11) 0.8225(7) 0.3971(7) 0.046(3) Uani 1 d . .
H17A H 0.4071(11) 0.8567(7) 0.4068(7) 0.055 Uiso 1 calc R .
C18 C 0.2859(10) 0.9954(6) 0.3265(7) 0.043(3) Uani 1 d . .
C19 C 0.2702(15) 0.9933(7) 0.4148(8) 0.069(4) Uani 1 d . .
H19A H 0.2466(15) 0.9491(7) 0.4385(8) 0.083 Uiso 1 calc R .
C20 C 0.2901(17) 1.0573(9) 0.4654(9) 0.089(6) Uani 1 d . .
H20A H 0.2804(17) 1.0556(9) 0.5237(9) 0.107 Uiso 1 calc R .
C21 C 0.3235(17) 1.1228(9) 0.4325(10) 0.088(6) Uani 1 d . .
H21A H 0.3358(17) 1.1655(9) 0.4680(10) 0.106 Uiso 1 calc R .
C22 C 0.3391(13) 1.1262(7) 0.3477(11) 0.069(4) Uani 1 d . .
H22A H 0.3639(13) 1.1706(7) 0.3252(11) 0.083 Uiso 1 calc R .
C23 C 0.3174(11) 1.0623(7) 0.2952(8) 0.051(3) Uani 1 d . .
H23A H 0.3248(11) 1.0654(7) 0.2365(8) 0.061 Uiso 1 calc R .
C24 C 0.1014(10) 0.9305(6) 0.2053(8) 0.044(3) Uani 1 d . .
C25 C 0.0583(11) 0.9332(7) 0.1150(8) 0.055(3) Uani 1 d . .
H25A H 0.1091(11) 0.9274(7) 0.0759(8) 0.066 Uiso 1 calc R .
C26 C -0.0594(12) 0.9445(9) 0.0827(10) 0.070(4) Uani 1 d . .
H26A H -0.0866(12) 0.9439(9) 0.0221(10) 0.084 Uiso 1 calc R .
C27 C -0.1363(12) 0.9564(9) 0.1378(11) 0.069(4) Uani 1 d . .
H27A H -0.2148(12) 0.9647(9) 0.1153(11) 0.083 Uiso 1 calc R .
C28 C -0.0950(11) 0.9557(8) 0.2278(10) 0.064(4) Uani 1 d . .
H28A H -0.1463(11) 0.9628(8) 0.2664(10) 0.077 Uiso 1 calc R .
C29 C 0.0213(11) 0.9446(8) 0.2604(9) 0.060(4) Uani 1 d . .
H29A H 0.0479(11) 0.9465(8) 0.3210(9) 0.072 Uiso 1 calc R .
C30 C 0.5167(24) 0.6658(11) 0.0299(12) 0.137(9) Uani 1 d . .
H30C H 0.5829(24) 0.6971(11) 0.0243(12) 0.165 Uiso 1 calc R .
H30A H 0.4762(24) 0.6907(11) 0.0711(12) 0.165 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'
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 74.2(4) . . y
N3 Re Cl2 101.1(3) . . y
N1 Re Cl2 175.2(3) . . y
N3 Re Cl3 165.4(3) . . y
N1 Re Cl3 91.5(3) . . y
Cl2 Re Cl3 93.26(11) . . y
N3 Re Cl1 88.9(3) . . y
N1 Re Cl1 89.8(2) . . y
Cl2 Re Cl1 91.07(12) . . y
Cl3 Re Cl1 88.40(13) . . y
N3 Re P1 94.8(3) . . y
N1 Re P1 91.7(2) . . y
Cl2 Re P1 87.70(10) . . y
Cl3 Re P1 88.14(12) . . y
Cl1 Re P1 176.26(11) . . y
C24 P1 C12 105.5(5) . . ?
C24 P1 C18 101.8(5) . . ?
C12 P1 C18 104.6(5) . . ?
C24 P1 Re 119.7(4) . . ?
C12 P1 Re 109.4(3) . . ?
C18 P1 Re 114.5(4) . . ?
C5 N1 C1 117.0(10) . . ?
C5 N1 Re 127.7(8) . . ?
C1 N1 Re 115.3(7) . . ?
N3 N2 C1 110.9(10) . . ?
N2 N3 C6 110.3(9) . . ?
N2 N3 Re 122.7(8) . . ?
C6 N3 Re 126.9(7) . . ?
N1 C1 N2 116.8(10) . . ?
N1 C1 C2 122.6(11) . . ?
N2 C1 C2 120.6(11) . . ?
C3 C2 C1 119.9(13) . . ?
C2 C3 C4 118.4(12) . . ?
C5 C4 C3 118.8(12) . . ?
N1 C5 C4 123.2(12) . . ?
C11 C6 C7 122.2(11) . . ?
C11 C6 N3 118.0(10) . . ?
C7 C6 N3 119.8(9) . . ?
C6 C7 C8 118.9(11) . . ?
C9 C8 C7 118.0(11) . . ?
C10 C9 C8 122.5(12) . . ?
C10 C9 Cl4 117.9(10) . . ?
C8 C9 Cl4 119.5(10) . . ?
C11 C10 C9 119.0(12) . . ?
C10 C11 C6 119.5(12) . . ?
C13 C12 C17 117.5(10) . . ?
C13 C12 P1 122.3(9) . . ?
C17 C12 P1 120.2(9) . . ?
C12 C13 C14 121.6(12) . . ?
C15 C14 C13 120.3(13) . . ?
C16 C15 C14 119.6(12) . . ?
C15 C16 C17 120.5(12) . . ?
C12 C17 C16 120.5(12) . . ?
C23 C18 C19 117.4(11) . . ?
C23 C18 P1 121.0(9) . . ?
C19 C18 P1 121.3(10) . . ?
C20 C19 C18 119.4(13) . . ?
C21 C20 C19 121.7(14) . . ?
C20 C21 C22 120.0(14) . . ?
C21 C22 C23 119.0(14) . . ?
C18 C23 C22 122.5(12) . . ?
C25 C24 C29 116.5(11) . . ?
C25 C24 P1 124.2(9) . . ?
C29 C24 P1 119.3(9) . . ?
C26 C25 C24 120.8(12) . . ?
C27 C26 C25 121.5(14) . . ?
C26 C27 C28 118.7(13) . . ?
C29 C28 C27 120.2(13) . . ?
C28 C29 C24 122.2(12) . . ?
Cl5 C30 Cl6 117.6(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 N3 1.994(10) . y
Re N1 2.077(9) . y
Re Cl2 2.332(3) . y
Re Cl3 2.370(3) . y
Re Cl1 2.375(3) . y
Re P1 2.510(3) . y
Cl4 C9 1.740(12) . ?
Cl5 C30 1.64(2) . ?
Cl6 C30 1.71(2) . ?
P1 C24 1.808(12) . ?
P1 C12 1.816(11) . ?
P1 C18 1.826(11) . ?
N1 C5 1.357(14) . ?
N1 C1 1.357(14) . ?
N2 N3 1.333(13) . y
N2 C1 1.369(15) . ?
N3 C6 1.467(15) . ?
C1 C2 1.38(2) . ?
C2 C3 1.36(2) . ?
C3 C4 1.41(2) . ?
C4 C5 1.37(2) . ?
C6 C11 1.377(15) . ?
C6 C7 1.379(15) . ?
C7 C8 1.40(2) . ?
C8 C9 1.39(2) . ?
C9 C10 1.38(2) . ?
C10 C11 1.38(2) . ?
C12 C13 1.38(2) . ?
C12 C17 1.40(2) . ?
C13 C14 1.38(2) . ?
C14 C15 1.37(2) . ?
C15 C16 1.36(2) . ?
C16 C17 1.40(2) . ?
C18 C23 1.36(2) . ?
C18 C19 1.41(2) . ?
C19 C20 1.37(2) . ?
C20 C21 1.36(2) . ?
C21 C22 1.36(2) . ?
C22 C23 1.39(2) . ?
C24 C25 1.39(2) . ?
C24 C29 1.40(2) . ?
C25 C26 1.39(2) . ?
C26 C27 1.37(2) . ?
C27 C28 1.38(2) . ?
C28 C29 1.37(2) . ?
