#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:37:03 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179069 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/31/4303105.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_4303105
loop_
_publ_author_name
'Ali Barandov'
'Ulrich Abram'
_publ_contact_author
;
      Ulrich Abram
      Free University of 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(V) Complexes with Pentadentate P,N,O Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8072
_journal_page_last               8074
_journal_paper_doi               10.1021/ic901152y
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C32 H25 Cl N2 O3 P Re'
_chemical_formula_sum            'C32 H25 Cl N2 O3 P Re'
_chemical_formula_weight         738.16
_chemical_name_common            '[ReCl(L2)].H2O'
_chemical_name_systematic
;
Chloro{bis(2-methylimino)phenolato)(phenyl)
phosphine}rhenium(V)
;
_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                106.93(1)
_cell_angle_beta                 90.90(1)
_cell_angle_gamma                108.46(1)
_cell_formula_units_Z            2
_cell_length_a                   8.763(1)
_cell_length_b                   11.019(1)
_cell_length_c                   15.830(2)
_cell_measurement_reflns_used    10464
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.67
_cell_measurement_theta_min      2.08
_cell_volume                     1377.2(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    Ortep3
_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 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.1239
_diffrn_reflns_av_sigmaI/netI    0.1397
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10016
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.47
_diffrn_standards_decay_%        0.1
_exptl_absorpt_coefficient_mu    4.602
_exptl_absorpt_correction_T_max  0.7803
_exptl_absorpt_correction_T_min  0.4536
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   X-red32
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.702
_refine_diff_density_min         -2.226
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.1037
_refine_ls_R_factor_gt           0.0617
_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)+(0.0621P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1412
_reflns_number_gt                3167
_reflns_number_total             4733
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901152y_si_002_3.cif
_cod_data_source_block           reclL2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4303105
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
Re Re 0.64794(6) 0.75250(5) 0.72851(4) 0.04555(19) Uani 1 1 d . . .
Cl Cl 0.5997(4) 0.9207(3) 0.8477(2) 0.0588(8) Uani 1 1 d . . .
P P 0.6022(3) 0.6225(3) 0.8261(2) 0.0463(8) Uani 1 1 d . . .
C1 C 0.6370(12) 0.4599(12) 0.7844(9) 0.048(3) Uani 1 1 d . . .
C2 C 0.6263(13) 0.3873(11) 0.8442(9) 0.050(3) Uani 1 1 d . . .
H2 H 0.6042 0.4222 0.9018 0.059 Uiso 1 1 calc R . .
C3 C 0.6482(13) 0.2642(12) 0.8181(9) 0.053(3) Uani 1 1 d . . .
H3 H 0.6418 0.2161 0.8582 0.063 Uiso 1 1 calc R . .
C4 C 0.6798(14) 0.2121(13) 0.7327(10) 0.059(4) Uani 1 1 d . . .
H4 H 0.6937 0.1285 0.7150 0.070 Uiso 1 1 calc R . .
C5 C 0.6908(13) 0.2838(12) 0.6728(9) 0.051(3) Uani 1 1 d . . .
H5 H 0.7134 0.2486 0.6153 0.061 Uiso 1 1 calc R . .
C6 C 0.6681(12) 0.4087(11) 0.6985(8) 0.044(3) Uani 1 1 d . . .
C7 C 0.6880(13) 0.4876(12) 0.6315(9) 0.047(3) Uani 1 1 d . . .
H7A H 0.8000 0.5455 0.6384 0.056 Uiso 1 1 calc R . .
H7B H 0.6627 0.4249 0.5716 0.056 Uiso 1 1 calc R . .
N1 N 0.5825(11) 0.5700(10) 0.6437(7) 0.049(2) Uani 1 1 d . . .
C11 C 0.4224(13) 0.5060(11) 0.6069(8) 0.045(3) Uani 1 1 d . . .
C12 C 0.3471(14) 0.3731(12) 0.5561(8) 0.052(3) Uani 1 1 d . . .
H12 H 0.4052 0.3139 0.5405 0.063 Uiso 1 1 calc R . .
C13 C 0.1834(15) 0.3310(14) 0.5292(9) 0.058(3) Uani 1 1 d . . .
H13 H 0.1302 0.2426 0.4941 0.070 Uiso 1 1 calc R . .
C14 C 0.0974(16) 0.4193(13) 0.5539(9) 0.058(3) Uani 1 1 d . . .
H14 H -0.0140 0.3862 0.5374 0.070 Uiso 1 1 calc R . .
C15 C 0.1676(14) 0.5519(12) 0.6012(9) 0.054(3) Uani 1 1 d . . .
H15 H 0.1092 0.6110 0.6136 0.065 Uiso 1 1 calc R . .
C16 C 0.3364(13) 0.5943(12) 0.6304(8) 0.045(3) Uani 1 1 d . . .
O1 O 0.4217(10) 0.7215(8) 0.6769(6) 0.053(2) Uani 1 1 d . . .
C21 C 0.7498(13) 0.7112(12) 0.9254(9) 0.050(3) Uani 1 1 d . . .
C22 C 0.7146(16) 0.7313(13) 1.0117(10) 0.063(4) Uani 1 1 d . . .
H22 H 0.6096 0.6908 1.0225 0.076 Uiso 1 1 calc R . .
C23 C 0.8308(17) 0.8093(13) 1.0819(9) 0.058(3) Uani 1 1 d . . .
H23 H 0.8047 0.8226 1.1398 0.070 Uiso 1 1 calc R . .
C24 C 0.9896(16) 0.8693(12) 1.0658(10) 0.061(4) Uani 1 1 d . . .
H24 H 1.0706 0.9215 1.1129 0.073 Uiso 1 1 calc R . .
C25 C 1.0239(14) 0.8499(12) 0.9797(10) 0.057(3) Uani 1 1 d . . .
H25 H 1.1290 0.8932 0.9703 0.069 Uiso 1 1 calc R . .
C26 C 0.9128(14) 0.7704(11) 0.9059(9) 0.049(3) Uani 1 1 d . . .
C27 C 0.9581(13) 0.7414(12) 0.8145(8) 0.045(3) Uani 1 1 d . . .
H27A H 1.0746 0.7815 0.8174 0.054 Uiso 1 1 calc R . .
H27B H 0.9303 0.6447 0.7885 0.054 Uiso 1 1 calc R . .
N2 N 0.8781(11) 0.7923(9) 0.7551(7) 0.047(2) Uani 1 1 d . . .
C31 C 0.9812(14) 0.8872(11) 0.7187(8) 0.044(3) Uani 1 1 d . . .
C32 C 1.1509(13) 0.9209(12) 0.7198(9) 0.053(3) Uani 1 1 d . . .
H32 H 1.2077 0.8828 0.7484 0.063 Uiso 1 1 calc R . .
C33 C 1.2319(17) 1.0137(15) 0.6764(12) 0.076(5) Uani 1 1 d . . .
H33 H 1.3440 1.0389 0.6779 0.092 Uiso 1 1 calc R . .
C34 C 1.1481(17) 1.0675(16) 0.6318(11) 0.075(5) Uani 1 1 d . . .
H34 H 1.2043 1.1263 0.6022 0.091 Uiso 1 1 calc R . .
C35 C 0.9822(16) 1.0360(12) 0.6302(9) 0.059(4) Uani 1 1 d . . .
H35 H 0.9266 1.0734 0.6003 0.070 Uiso 1 1 calc R . .
C36 C 0.8972(15) 0.9438(12) 0.6760(10) 0.058(3) Uani 1 1 d . . .
O2 O 0.7359(9) 0.9027(8) 0.6723(6) 0.053(2) Uani 1 1 d . . .
C41 C 0.3981(13) 0.5720(12) 0.8565(9) 0.049(3) Uani 1 1 d . . .
C42 C 0.2887(14) 0.4514(14) 0.8028(9) 0.055(3) Uani 1 1 d . . .
H42 H 0.3242 0.3959 0.7570 0.066 Uiso 1 1 calc R . .
C43 C 0.1255(16) 0.4123(16) 0.8165(11) 0.071(4) Uani 1 1 d . . .
H43 H 0.0512 0.3332 0.7788 0.085 Uiso 1 1 calc R . .
C44 C 0.0771(17) 0.4923(18) 0.8865(12) 0.073(4) Uani 1 1 d . . .
H44 H -0.0304 0.4648 0.8975 0.088 Uiso 1 1 calc R . .
C45 C 0.1838(17) 0.6132(17) 0.9413(11) 0.072(4) Uani 1 1 d . . .
H45 H 0.1487 0.6661 0.9888 0.087 Uiso 1 1 calc R . .
C46 C 0.3441(15) 0.6544(14) 0.9243(10) 0.058(3) Uani 1 1 d . . .
H46 H 0.4156 0.7377 0.9587 0.070 Uiso 1 1 calc R . .
O3 O 0.497(2) 0.1133(13) 0.4657(11) 0.048(4) Uani 0.50 1 d P . .
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
N2 Re N1 101.8(4) . . ?
N2 Re O1 167.7(4) . . ?
N1 Re O1 76.3(4) . . ?
N2 Re O2 80.2(4) . . ?
N1 Re O2 114.2(4) . . ?
O1 Re O2 89.4(3) . . ?
N2 Re P 88.5(3) . . ?
N1 Re P 79.1(3) . . ?
O1 Re P 103.0(2) . . ?
O2 Re P 163.9(3) . . ?
N2 Re Cl 101.2(3) . . ?
N1 Re Cl 151.8(3) . . ?
O1 Re Cl 84.4(3) . . ?
O2 Re Cl 85.6(3) . . ?
P Re Cl 85.42(12) . . ?
C21 P C41 110.6(6) . . ?
C21 P C1 102.7(6) . . ?
C41 P C1 102.1(5) . . ?
C21 P Re 109.2(4) . . ?
C41 P Re 116.0(4) . . ?
C1 P Re 115.3(4) . . ?
C6 C1 C2 120.6(11) . . ?
C6 C1 P 123.2(10) . . ?
C2 C1 P 116.3(10) . . ?
C3 C2 C1 120.0(12) . . ?
C2 C3 C4 120.0(13) . . ?
C3 C4 C5 120.3(13) . . ?
C4 C5 C6 120.1(13) . . ?
C1 C6 C5 119.0(11) . . ?
C1 C6 C7 122.3(11) . . ?
C5 C6 C7 118.6(11) . . ?
N1 C7 C6 112.0(9) . . ?
C11 N1 C7 117.3(10) . . ?
C11 N1 Re 119.4(8) . . ?
C7 N1 Re 122.1(7) . . ?
C12 C11 N1 128.5(12) . . ?
C12 C11 C16 121.2(11) . . ?
N1 C11 C16 110.2(10) . . ?
C11 C12 C13 117.9(13) . . ?
C14 C13 C12 120.7(12) . . ?
C15 C14 C13 123.3(12) . . ?
C14 C15 C16 115.7(13) . . ?
O1 C16 C11 116.4(10) . . ?
O1 C16 C15 122.5(11) . . ?
C11 C16 C15 121.0(11) . . ?
C16 O1 Re 115.5(7) . . ?
C22 C21 C26 120.9(12) . . ?
C22 C21 P 125.5(9) . . ?
C26 C21 P 113.4(9) . . ?
C21 C22 C23 121.4(12) . . ?
C22 C23 C24 119.4(13) . . ?
C25 C24 C23 119.0(12) . . ?
C24 C25 C26 124.4(12) . . ?
C25 C26 C21 114.8(12) . . ?
C25 C26 C27 122.7(11) . . ?
C21 C26 C27 122.4(11) . . ?
N2 C27 C26 114.1(10) . . ?
C31 N2 C27 116.8(9) . . ?
C31 N2 Re 116.0(8) . . ?
C27 N2 Re 127.1(7) . . ?
C36 C31 N2 112.7(10) . . ?
C36 C31 C32 120.7(11) . . ?
N2 C31 C32 126.6(11) . . ?
C33 C32 C31 118.3(13) . . ?
C34 C33 C32 121.1(13) . . ?
C33 C34 C35 121.4(13) . . ?
C34 C35 C36 118.5(14) . . ?
C31 C36 O2 118.4(11) . . ?
C31 C36 C35 120.0(12) . . ?
O2 C36 C35 121.4(13) . . ?
C36 O2 Re 112.4(8) . . ?
C46 C41 C42 119.3(11) . . ?
C46 C41 P 123.0(9) . . ?
C42 C41 P 117.3(10) . . ?
C41 C42 C43 120.7(14) . . ?
C44 C43 C42 118.8(14) . . ?
C43 C44 C45 121.8(13) . . ?
C44 C45 C46 119.0(14) . . ?
C41 C46 C45 120.4(13) . . ?
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 N2 1.935(10) . ?
Re N1 1.961(10) . ?
Re O1 2.018(9) . ?
Re O2 2.048(8) . ?
Re P 2.354(3) . ?
Re Cl 2.379(3) . ?
P C21 1.827(13) . ?
P C41 1.815(11) . ?
P C1 1.845(13) . ?
C1 C6 1.379(17) . ?
C1 C2 1.393(17) . ?
C2 C3 1.375(17) . ?
C3 C4 1.377(19) . ?
C4 C5 1.387(18) . ?
C5 C6 1.396(17) . ?
C6 C7 1.536(16) . ?
C7 N1 1.467(15) . ?
N1 C11 1.383(14) . ?
C11 C12 1.383(16) . ?
C11 C16 1.384(17) . ?
C12 C13 1.378(17) . ?
C13 C14 1.39(2) . ?
C14 C15 1.361(17) . ?
C15 C16 1.426(17) . ?
C16 O1 1.336(14) . ?
C21 C22 1.375(18) . ?
C21 C26 1.449(16) . ?
C22 C23 1.365(19) . ?
C23 C24 1.402(18) . ?
C24 C25 1.370(19) . ?
C25 C26 1.381(17) . ?
C26 C27 1.477(17) . ?
C27 N2 1.492(16) . ?
N2 C31 1.419(14) . ?
C31 C36 1.381(18) . ?
C31 C32 1.412(16) . ?
C32 C33 1.409(18) . ?
C33 C34 1.37(2) . ?
C34 C35 1.382(19) . ?
C35 C36 1.442(17) . ?
C36 O2 1.335(14) . ?
C41 C46 1.386(18) . ?
C41 C42 1.385(17) . ?
C42 C43 1.398(17) . ?
C43 C44 1.37(2) . ?
C44 C45 1.38(2) . ?
C45 C46 1.390(18) . ?
