#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/16/4311676.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_4311676
loop_
_publ_author_name
'Lihui Wei'
'John W. Babich'
'Jon Zubieta'
_publ_contact_author_address
;Department of Chemistry
1-014 CST
Syracuse University
111 College Place
Syracuse, NY 13244
;
_publ_contact_author_email       jazubiet@syr.edu
_publ_contact_author_fax         315-443-4070
_publ_contact_author_name        'Jon Zubieta'
_publ_contact_author_phone       315-443-2547
_publ_section_title
;
 Unusual Reactivity of the {ReVO}3+ Core: Syntheses and Characterization
 of Novel Rhenium Halide Complexes with N-Methyl-o-diaminobenzene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6445
_journal_page_last               6454
_journal_paper_doi               10.1021/ic049372p
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C18 H15 Cl2 O P Re0.5'
_chemical_formula_weight         442.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.0950(10)
_cell_angle_beta                 108.2160(10)
_cell_angle_gamma                93.8760(10)
_cell_formula_units_Z            2
_cell_length_a                   9.2986(6)
_cell_length_b                   9.6486(6)
_cell_length_c                   10.3467(7)
_cell_measurement_reflns_used    5579
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.51
_cell_measurement_theta_min      2.14
_cell_volume                     853.30(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Platfrom w/APEX CCD detector'
_diffrn_measurement_method       'Phi and omega 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  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0938
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11237
_diffrn_reflns_theta_full        31.51
_diffrn_reflns_theta_max         31.51
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    4.000
_exptl_absorpt_correction_T_max  0.8564
_exptl_absorpt_correction_T_min  0.7953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 97)'
_exptl_crystal_colour            res
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             435
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.250
_refine_diff_density_min         -1.360
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         5579
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0465P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1084
_reflns_number_gt                4843
_reflns_number_total             5579
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049372psi20040712_033522.cif
_cod_data_source_block           p-1
_cod_original_formula_sum        'C18 H15 Cl2 O P Re0.50'
_cod_database_code               4311676
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.0000 0.0000 0.5000 0.01765(9) Uani 1 2 d S . .
Cl1 Cl -0.14396(14) -0.05724(14) 0.63683(13) 0.0263(3) Uani 1 1 d . . .
Cl2 Cl -0.19044(14) 0.12532(14) 0.39117(13) 0.0271(3) Uani 1 1 d . . .
P1 P 0.23143(15) 0.27783(15) 0.75986(14) 0.0256(3) Uani 1 1 d . . .
O1 O 0.1000(4) 0.1824(4) 0.6473(4) 0.0309(8) Uani 1 1 d . . .
C1 C 0.1616(6) 0.4420(6) 0.8121(6) 0.0275(11) Uani 1 1 d . . .
C2 C 0.0652(6) 0.4931(6) 0.7038(6) 0.0317(12) Uani 1 1 d . . .
H2 H 0.0379 0.4417 0.6109 0.038 Uiso 1 1 calc R . .
C3 C 0.0112(7) 0.6214(7) 0.7374(8) 0.0418(15) Uani 1 1 d . . .
H3 H -0.0515 0.6578 0.6669 0.050 Uiso 1 1 calc R . .
C4 C 0.0506(7) 0.6945(7) 0.8751(7) 0.0414(15) Uani 1 1 d . . .
H4 H 0.0133 0.7802 0.8969 0.050 Uiso 1 1 calc R . .
C5 C 0.1443(7) 0.6439(7) 0.9825(7) 0.0422(15) Uani 1 1 d . . .
H5 H 0.1700 0.6952 1.0753 0.051 Uiso 1 1 calc R . .
C6 C 0.1994(7) 0.5161(7) 0.9504(6) 0.0346(13) Uani 1 1 d . . .
H6 H 0.2616 0.4803 1.0216 0.042 Uiso 1 1 calc R . .
C7 C 0.3000(6) 0.2022(6) 0.9066(5) 0.0276(11) Uani 1 1 d . . .
C8 C 0.1976(7) 0.1192(7) 0.9432(6) 0.0329(13) Uani 1 1 d . . .
H8 H 0.0950 0.0973 0.8876 0.040 Uiso 1 1 calc R . .
C9 C 0.2512(7) 0.0693(7) 1.0646(6) 0.0356(13) Uani 1 1 d . . .
H9 H 0.1839 0.0137 1.0900 0.043 Uiso 1 1 calc R . .
C10 C 0.4023(7) 0.1017(6) 1.1465(6) 0.0375(14) Uani 1 1 d . . .
H10 H 0.4360 0.0720 1.2295 0.045 Uiso 1 1 calc R . .
C11 C 0.5039(7) 0.1777(7) 1.1068(6) 0.0379(14) Uani 1 1 d . . .
H11 H 0.6073 0.1949 1.1603 0.046 Uiso 1 1 calc R . .
C12 C 0.4533(6) 0.2290(7) 0.9873(6) 0.0351(13) Uani 1 1 d . . .
H12 H 0.5225 0.2815 0.9614 0.042 Uiso 1 1 calc R . .
C13 C 0.3880(6) 0.3153(6) 0.7015(5) 0.0276(11) Uani 1 1 d . . .
C14 C 0.4590(6) 0.1999(7) 0.6546(6) 0.0319(12) Uani 1 1 d . . .
H14 H 0.4212 0.1067 0.6504 0.038 Uiso 1 1 calc R . .
C15 C 0.5854(6) 0.2257(7) 0.6145(6) 0.0346(13) Uani 1 1 d . . .
H15 H 0.6325 0.1499 0.5830 0.041 Uiso 1 1 calc R . .
C16 C 0.6405(7) 0.3633(7) 0.6214(7) 0.0426(15) Uani 1 1 d . . .
H16 H 0.7255 0.3806 0.5949 0.051 Uiso 1 1 calc R . .
C17 C 0.5717(7) 0.4756(8) 0.6670(7) 0.0420(15) Uani 1 1 d . . .
H17 H 0.6109 0.5685 0.6716 0.050 Uiso 1 1 calc R . .
C18 C 0.4445(7) 0.4525(7) 0.7063(6) 0.0367(13) Uani 1 1 d . . .
H18 H 0.3975 0.5292 0.7357 0.044 Uiso 1 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'
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
O1 Re1 O1 180.0 . 2_556 ?
O1 Re1 Cl2 88.79(11) . . ?
O1 Re1 Cl2 91.21(11) 2_556 . ?
O1 Re1 Cl2 91.21(11) . 2_556 ?
O1 Re1 Cl2 88.79(11) 2_556 2_556 ?
Cl2 Re1 Cl2 179.999(2) . 2_556 ?
O1 Re1 Cl1 89.83(11) . . ?
O1 Re1 Cl1 90.17(11) 2_556 . ?
Cl2 Re1 Cl1 90.26(4) . . ?
Cl2 Re1 Cl1 89.74(4) 2_556 . ?
O1 Re1 Cl1 90.17(11) . 2_556 ?
O1 Re1 Cl1 89.83(11) 2_556 2_556 ?
Cl2 Re1 Cl1 89.74(4) . 2_556 ?
Cl2 Re1 Cl1 90.26(4) 2_556 2_556 ?
Cl1 Re1 Cl1 180.0 . 2_556 ?
O1 P1 C7 111.5(3) . . ?
O1 P1 C13 112.6(2) . . ?
C7 P1 C13 107.8(2) . . ?
O1 P1 C1 106.2(2) . . ?
C7 P1 C1 109.6(3) . . ?
C13 P1 C1 109.1(3) . . ?
P1 O1 Re1 153.9(3) . . ?
C6 C1 C2 120.8(5) . . ?
C6 C1 P1 122.9(4) . . ?
C2 C1 P1 116.3(4) . . ?
C3 C2 C1 118.9(6) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?
C4 C3 C2 119.7(6) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 121.6(6) . . ?
C3 C4 H4 119.2 . . ?
C5 C4 H4 119.2 . . ?
C4 C5 C6 119.2(6) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C1 C6 C5 119.7(6) . . ?
C1 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
C12 C7 C8 119.7(5) . . ?
C12 C7 P1 120.6(4) . . ?
C8 C7 P1 119.7(4) . . ?
C7 C8 C9 119.1(5) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 H8 120.4 . . ?
C10 C9 C8 120.4(5) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C11 C10 C9 120.4(5) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C10 C11 C12 120.2(6) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C7 C12 C11 120.1(6) . . ?
C7 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C18 C13 C14 119.5(5) . . ?
C18 C13 P1 122.3(4) . . ?
C14 C13 P1 118.2(4) . . ?
C15 C14 C13 119.8(5) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C16 C15 C14 119.7(6) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
C17 C16 C15 120.7(6) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C16 C17 C18 120.7(6) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C13 C18 C17 119.7(6) . . ?
C13 C18 H18 120.2 . . ?
C17 C18 H18 120.2 . . ?
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
Re1 O1 2.013(4) . ?
Re1 O1 2.013(4) 2_556 ?
Re1 Cl2 2.3408(11) . ?
Re1 Cl2 2.3408(11) 2_556 ?
Re1 Cl1 2.3482(11) . ?
Re1 Cl1 2.3482(11) 2_556 ?
P1 O1 1.485(4) . ?
P1 C7 1.779(5) . ?
P1 C13 1.785(5) . ?
P1 C1 1.795(5) . ?
C1 C6 1.380(8) . ?
C1 C2 1.402(7) . ?
C2 C3 1.385(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.371(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.382(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.383(8) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C12 1.383(8) . ?
C7 C8 1.393(8) . ?
C8 C9 1.398(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.369(9) . ?
C9 H9 0.9300 . ?
C10 C11 1.369(9) . ?
C10 H10 0.9300 . ?
C11 C12 1.386(8) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C18 1.376(8) . ?
C13 C14 1.409(7) . ?
C14 C15 1.387(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.370(9) . ?
C15 H15 0.9300 . ?
C16 C17 1.369(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.385(8) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 P1 O1 Re1 -63.3(6) . . . . ?
C13 P1 O1 Re1 58.1(6) . . . . ?
C1 P1 O1 Re1 177.4(5) . . . . ?
O1 Re1 O1 P1 -16(5) 2_556 . . . ?
Cl2 Re1 O1 P1 -158.1(5) . . . . ?
Cl2 Re1 O1 P1 21.9(5) 2_556 . . . ?
Cl1 Re1 O1 P1 111.6(5) . . . . ?
Cl1 Re1 O1 P1 -68.4(5) 2_556 . . . ?
O1 P1 C1 C6 138.5(5) . . . . ?
C7 P1 C1 C6 18.0(6) . . . . ?
C13 P1 C1 C6 -99.9(5) . . . . ?
O1 P1 C1 C2 -41.7(5) . . . . ?
C7 P1 C1 C2 -162.3(4) . . . . ?
C13 P1 C1 C2 79.8(5) . . . . ?
C6 C1 C2 C3 1.6(8) . . . . ?
P1 C1 C2 C3 -178.2(4) . . . . ?
C1 C2 C3 C4 -1.1(9) . . . . ?
C2 C3 C4 C5 0.4(10) . . . . ?
C3 C4 C5 C6 -0.2(10) . . . . ?
C2 C1 C6 C5 -1.4(9) . . . . ?
P1 C1 C6 C5 178.4(5) . . . . ?
C4 C5 C6 C1 0.7(9) . . . . ?
O1 P1 C7 C12 148.1(5) . . . . ?
C13 P1 C7 C12 24.1(6) . . . . ?
C1 P1 C7 C12 -94.6(5) . . . . ?
O1 P1 C7 C8 -34.0(5) . . . . ?
C13 P1 C7 C8 -158.1(5) . . . . ?
C1 P1 C7 C8 83.3(5) . . . . ?
C12 C7 C8 C9 2.6(9) . . . . ?
P1 C7 C8 C9 -175.3(5) . . . . ?
C7 C8 C9 C10 0.1(9) . . . . ?
C8 C9 C10 C11 -3.1(9) . . . . ?
C9 C10 C11 C12 3.5(9) . . . . ?
C8 C7 C12 C11 -2.2(9) . . . . ?
P1 C7 C12 C11 175.6(5) . . . . ?
C10 C11 C12 C7 -0.8(9) . . . . ?
O1 P1 C13 C18 120.7(5) . . . . ?
C7 P1 C13 C18 -115.9(5) . . . . ?
C1 P1 C13 C18 3.1(6) . . . . ?
O1 P1 C13 C14 -61.9(5) . . . . ?
C7 P1 C13 C14 61.6(5) . . . . ?
C1 P1 C13 C14 -179.5(4) . . . . ?
C18 C13 C14 C15 0.4(8) . . . . ?
P1 C13 C14 C15 -177.1(4) . . . . ?
C13 C14 C15 C16 0.2(9) . . . . ?
C14 C15 C16 C17 -0.3(10) . . . . ?
C15 C16 C17 C18 -0.4(10) . . . . ?
C14 C13 C18 C17 -1.1(9) . . . . ?
P1 C13 C18 C17 176.4(5) . . . . ?
C16 C17 C18 C13 1.0(10) . . . . ?
