#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/70/4317095.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_4317095
loop_
_publ_author_name
'Jennifer Schroer'
'Stefan Wagner'
'Ulrich Abram'
_publ_contact_author
;
      Ulrich Abram
      Freie Universitaet  Berlin     
      Institute of Chemistry             
      Fabeckstrasse 34-36                     
      D-14195 Berlin         
      Germany                          
;
_publ_contact_author_email       abram@chemie.fu-berlin.de
_publ_contact_author_fax         '0049 (0)30 838 52676'
_publ_contact_author_phone       '0049 (0)30 838 54002'
_publ_section_title
;
 Rhenium Complexes with 2-(Diphenylphosphinomethyl)aniline: Formation of a
 Cyclic, Trinuclear Oxorhenium(V) Core
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10694
_journal_page_last               10701
_journal_paper_doi               10.1021/ic101792j
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C19 H18 Cl3 N O P Re'
_chemical_formula_sum            'C19 H18 Cl3 N O P Re'
_chemical_formula_weight         599.86
_chemical_name_common            '[ReO(H2L2)Cl3]'
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.640(10)
_cell_angle_beta                 103.780(10)
_cell_angle_gamma                114.200(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4480(10)
_cell_length_b                   9.9130(10)
_cell_length_c                   13.0750(10)
_cell_measurement_reflns_used    12080
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.59
_cell_measurement_theta_min      2.39
_cell_volume                     1021.0(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    oRTEP3
_computing_publication_material  WingGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXs-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.0683
_diffrn_reflns_av_sigmaI/netI    0.0613
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11171
_diffrn_reflns_theta_full        29.24
_diffrn_reflns_theta_max         29.24
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        0.1
_exptl_absorpt_coefficient_mu    6.430
_exptl_absorpt_correction_T_max  0.7157
_exptl_absorpt_correction_T_min  0.6007
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-Red 32'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.951
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.704
_refine_diff_density_min         -1.657
_refine_diff_density_rms         0.235
_refine_ls_extinction_coef       0.0147(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         5438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0521
_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)+(0.0351P)²+14.6057P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1422
_reflns_number_gt                4520
_reflns_number_total             5438
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101792j_si_002_5.cif
_cod_data_source_block           jsrepn1
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4317095
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 0.52966(5) 0.56864(5) 0.73340(3) 0.03205(15) Uani 1 1 d . . .
O10 O 0.6224(10) 0.7565(9) 0.8155(7) 0.0449(17) Uani 1 1 d . . .
Cl3 Cl 0.3430(3) 0.3147(3) 0.58366(19) 0.0366(5) Uani 1 1 d . . .
Cl2 Cl 0.5926(4) 0.4427(4) 0.8543(2) 0.0496(6) Uani 1 1 d . . .
Cl1 Cl 0.7476(3) 0.5656(3) 0.6714(2) 0.0425(5) Uani 1 1 d . . .
P1 P 0.2637(3) 0.5102(3) 0.7556(2) 0.0313(5) Uani 1 1 d . . .
C1 C 0.1428(12) 0.5359(11) 0.6353(8) 0.0347(19) Uani 1 1 d . . .
H1C H 0.1236 0.4608 0.5663 0.042 Uiso 1 1 calc R . .
H1D H 0.0357 0.5169 0.6400 0.042 Uiso 1 1 calc R . .
C11 C 0.2362(12) 0.6996(11) 0.6351(8) 0.0351(19) Uani 1 1 d . . .
C12 C 0.1802(14) 0.8082(13) 0.6572(9) 0.043(2) Uani 1 1 d . . .
H12 H 0.0821 0.7781 0.6718 0.051 Uiso 1 1 calc R . .
C13 C 0.2675(15) 0.9605(14) 0.6580(11) 0.049(3) Uani 1 1 d . . .
H13 H 0.2263 1.0303 0.6716 0.059 Uiso 1 1 calc R . .
C14 C 0.4142(16) 1.0084(14) 0.6390(11) 0.049(3) Uani 1 1 d . . .
H14 H 0.4731 1.1110 0.6407 0.059 Uiso 1 1 calc R . .
C15 C 0.4748(14) 0.9042(13) 0.6170(10) 0.045(2) Uani 1 1 d . . .
H15 H 0.5745 0.9368 0.6045 0.053 Uiso 1 1 calc R . .
C16 C 0.3863(12) 0.7520(12) 0.6140(8) 0.0358(19) Uani 1 1 d . . .
N1 N 0.4527(11) 0.6442(10) 0.5952(7) 0.0367(17) Uani 1 1 d . . .
H1A H 0.5410 0.6900 0.5753 0.044 Uiso 1 1 calc R . .
H1B H 0.3750 0.5579 0.5366 0.044 Uiso 1 1 calc R . .
C21 C 0.1429(12) 0.3148(10) 0.7578(9) 0.037(2) Uani 1 1 d . . .
C22 C 0.0138(13) 0.1955(13) 0.6631(10) 0.048(3) Uani 1 1 d . . .
H22 H -0.0164 0.2141 0.5964 0.058 Uiso 1 1 calc R . .
C23 C -0.0723(16) 0.0418(14) 0.6710(15) 0.071(5) Uani 1 1 d . . .
H23 H -0.1611 -0.0403 0.6098 0.085 Uiso 1 1 calc R . .
C24 C -0.0218(19) 0.0190(16) 0.7693(14) 0.064(4) Uani 1 1 d . . .
H24 H -0.0754 -0.0804 0.7743 0.077 Uiso 1 1 calc R . .
C25 C 0.1028(18) 0.1355(14) 0.8584(13) 0.059(3) Uani 1 1 d . . .
H25 H 0.1330 0.1158 0.9246 0.070 Uiso 1 1 calc R . .
C26 C 0.1873(15) 0.2828(12) 0.8557(10) 0.043(2) Uani 1 1 d . . .
H26 H 0.2745 0.3620 0.9192 0.052 Uiso 1 1 calc R . .
C31 C 0.2636(13) 0.6376(11) 0.8777(8) 0.0352(19) Uani 1 1 d . . .
C32 C 0.4039(15) 0.7601(12) 0.9600(9) 0.046(2) Uani 1 1 d . . .
H32 H 0.5075 0.7817 0.9560 0.055 Uiso 1 1 calc R . .
C33 C 0.3928(18) 0.8536(14) 1.0507(10) 0.055(3) Uani 1 1 d . . .
H33 H 0.4883 0.9362 1.1073 0.066 Uiso 1 1 calc R . .
C34 C 0.2385(19) 0.8212(15) 1.0542(10) 0.057(3) Uani 1 1 d . . .
H34 H 0.2301 0.8843 1.1131 0.068 Uiso 1 1 calc R . .
C35 C 0.0962(19) 0.6971(19) 0.9724(13) 0.068(4) Uani 1 1 d . . .
H35 H -0.0073 0.6764 0.9765 0.081 Uiso 1 1 calc R . .
C36 C 0.1070(15) 0.6045(15) 0.8853(10) 0.051(3) Uani 1 1 d . . .
H36 H 0.0110 0.5194 0.8308 0.061 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'
Cl Cl 0.1484 0.1585 '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'
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
O10 Re1 N1 87.1(4) . . ?
O10 Re1 Cl2 103.7(3) . . ?
N1 Re1 Cl2 169.0(2) . . ?
O10 Re1 Cl1 100.5(3) . . ?
N1 Re1 Cl1 88.2(2) . . ?
Cl2 Re1 Cl1 88.05(10) . . ?
O10 Re1 P1 93.4(3) . . ?
N1 Re1 P1 88.0(2) . . ?
Cl2 Re1 P1 92.99(10) . . ?
Cl1 Re1 P1 165.37(8) . . ?
O10 Re1 Cl3 164.3(3) . . ?
N1 Re1 Cl3 79.1(2) . . ?
Cl2 Re1 Cl3 90.39(10) . . ?
Cl1 Re1 Cl3 86.76(9) . . ?
P1 Re1 Cl3 78.64(8) . . ?
C21 P1 C31 103.3(5) . . ?
C21 P1 C1 108.5(5) . . ?
C31 P1 C1 104.5(4) . . ?
C21 P1 Re1 116.1(3) . . ?
C31 P1 Re1 118.2(4) . . ?
C1 P1 Re1 105.5(3) . . ?
C11 C1 P1 109.5(7) . . ?
C12 C11 C16 116.8(9) . . ?
C12 C11 C1 121.5(9) . . ?
C16 C11 C1 121.8(8) . . ?
C13 C12 C11 121.5(10) . . ?
C14 C13 C12 120.2(10) . . ?
C13 C14 C15 120.2(11) . . ?
C16 C15 C14 119.6(10) . . ?
C15 C16 C11 121.7(9) . . ?
C15 C16 N1 119.7(9) . . ?
C11 C16 N1 118.5(9) . . ?
C16 N1 Re1 117.3(6) . . ?
C22 C21 C26 119.7(10) . . ?
C22 C21 P1 121.7(9) . . ?
C26 C21 P1 118.6(8) . . ?
C21 C22 C23 118.1(13) . . ?
C24 C23 C22 119.0(12) . . ?
C25 C24 C23 121.4(12) . . ?
C24 C25 C26 122.0(14) . . ?
C25 C26 C21 119.8(12) . . ?
C32 C31 C36 119.3(9) . . ?
C32 C31 P1 124.0(8) . . ?
C36 C31 P1 116.7(8) . . ?
C31 C32 C33 120.5(12) . . ?
C34 C33 C32 118.9(12) . . ?
C33 C34 C35 121.2(10) . . ?
C36 C35 C34 119.9(13) . . ?
C35 C36 C31 120.2(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
Re1 O10 1.672(7) . ?
Re1 N1 2.173(8) . ?
Re1 Cl2 2.317(3) . ?
Re1 Cl1 2.394(2) . ?
Re1 P1 2.440(2) . ?
Re1 Cl3 2.451(2) . ?
P1 C21 1.812(10) . ?
P1 C31 1.825(9) . ?
P1 C1 1.841(10) . ?
C1 C11 1.497(14) . ?
C11 C12 1.392(13) . ?
C11 C16 1.414(14) . ?
C12 C13 1.389(17) . ?
C13 C14 1.372(16) . ?
C14 C15 1.386(14) . ?
C15 C16 1.379(15) . ?
C16 N1 1.454(12) . ?
C21 C22 1.389(14) . ?
C21 C26 1.390(15) . ?
C22 C23 1.442(19) . ?
C23 C24 1.36(2) . ?
C24 C25 1.33(2) . ?
C25 C26 1.360(15) . ?
C31 C32 1.365(15) . ?
C31 C36 1.411(15) . ?
C32 C33 1.404(15) . ?
C33 C34 1.372(19) . ?
C34 C35 1.38(2) . ?
C35 C36 1.365(16) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Cl3 0.90 2.57 3.354(9) 145.8 2_666
N1 H1B Cl1 0.90 2.50 3.281(9) 145.9 2_666
