#------------------------------------------------------------------------------
#$Date: 2019-11-23 05:33:27 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232236 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/72/4347249.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_4347249
loop_
_publ_author_name
'Liu, Jinyong'
'Wu, Dimao'
'Su, Xiaoge'
'Han, Mengwei'
'Kimura, Susana Y.'
'Gray, Danielle L.'
'Shapley, John R.'
'Abu-Omar, Mahdi M'
'Werth, Charles J.'
'Strathmann, Timothy J.'
_publ_section_title
;
 Configuration Control in the Synthesis of Homo- and Heteroleptic
 Bis(oxazolinylphenolato/thiazolinylphenolato) Chelate Ligand Complexes of
 Oxorhenium(V): Isomer Effect on Ancillary Ligand Exchange Dynamics and
 Implications for Perchlorate Reduction Catalysis.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2597
_journal_page_last               2611
_journal_paper_doi               10.1021/acs.inorgchem.5b02940
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C9 H8 Cl3 N O3 Re, C9 H10 N O2'
_chemical_formula_sum            'C18 H18 Cl3 N2 O5 Re'
_chemical_formula_weight         634.89
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
? 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.1360(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8742(8)
_cell_length_b                   15.0566(12)
_cell_length_c                   13.6439(11)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    188(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.47
_cell_volume                     2028.5(3)
_computing_cell_refinement       'SAINT V7.68A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2010.11-3 (Bruker, 2010)'
_computing_data_reduction
; 
SAINT V7.68A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5 
(Bruker, 2005 & 2007) 
;
_computing_molecular_graphics
; 
SHELXTL V6.12 (Bruker, 2005), CrystalMaker v2.1.3 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      188(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Siemens Platform/ApexII CCD'
_diffrn_measurement_method       'profile data from ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  bm90vas
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24087
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    6.419
_exptl_absorpt_correction_T_max  0.7524
_exptl_absorpt_correction_T_min  0.2258
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.079
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1224
_exptl_crystal_id                bm90vas
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (3 2 0) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         4160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0164
_refine_ls_R_factor_gt           0.0152
_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)+(0.0175P)²+1.1071P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0366
_refine_ls_wR_factor_ref         0.0372
_reflns_number_gt                3971
_reflns_number_total             4160
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02940_si_002.cif
_cod_data_source_block           '[H2hoz][Re(O)(hoz)Cl3]_(3)'
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P2(1)/c  '
_cod_database_code               4347249
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Re1 Re 0.667981(9) 0.051643(6) 0.220080(7) 0.01742(4) Uani 1 1 d .
Cl1 Cl 0.78080(6) 0.06871(4) 0.05979(5) 0.02480(13) Uani 1 1 d .
Cl2 Cl 0.64716(6) 0.20769(4) 0.23637(5) 0.02836(14) Uani 1 1 d .
Cl3 Cl 0.58205(7) 0.03545(4) 0.38051(5) 0.02844(14) Uani 1 1 d .
O1 O 0.52519(16) 0.02643(11) 0.15833(13) 0.0247(4) Uani 1 1 d .
O2 O 0.85530(16) 0.06236(10) 0.27036(13) 0.0215(4) Uani 1 1 d .
O3 O 0.83631(16) -0.21033(10) 0.23487(13) 0.0246(4) Uani 1 1 d .
N1 N 0.71856(19) -0.08365(12) 0.22471(14) 0.0179(4) Uani 1 1 d .
C1 C 0.9688(2) 0.01605(16) 0.25414(18) 0.0205(5) Uani 1 1 d .
C2 C 0.9662(2) -0.07571(15) 0.23390(18) 0.0201(5) Uani 1 1 d .
C3 C 1.0879(2) -0.12161(17) 0.22002(19) 0.0255(5) Uani 1 1 d .
H3 H 1.0864 -0.1837 0.2075 0.031 Uiso 1 1 calc R
C4 C 1.2102(3) -0.07717(19) 0.2244(2) 0.0316(6) Uani 1 1 d .
H4 H 1.2924 -0.1084 0.2135 0.038 Uiso 1 1 calc R
C5 C 1.2128(3) 0.01341(18) 0.2448(2) 0.0316(6) Uani 1 1 d .
H5 H 1.2971 0.0437 0.2476 0.038 Uiso 1 1 calc R
C6 C 1.0940(3) 0.05984(16) 0.2609(2) 0.0267(6) Uani 1 1 d .
H6 H 1.0972 0.1213 0.2765 0.032 Uiso 1 1 calc R
C7 C 0.8362(2) -0.12084(15) 0.22984(17) 0.0187(5) Uani 1 1 d .
C8 C 0.6941(2) -0.23962(16) 0.23206(19) 0.0223(5) Uani 1 1 d .
H8A H 0.6720 -0.2758 0.2904 0.027 Uiso 1 1 calc R
H8B H 0.6757 -0.2751 0.1724 0.027 Uiso 1 1 calc R
C9 C 0.6117(2) -0.15311(15) 0.23118(18) 0.0205(5) Uani 1 1 d .
H9A H 0.5501 -0.1507 0.1739 0.025 Uiso 1 1 calc R
H9B H 0.5580 -0.1466 0.2919 0.025 Uiso 1 1 calc R
O4 O 0.89598(18) 0.88360(12) 0.99271(15) 0.0282(4) Uani 1 1 d .
H4A H 0.868(4) 0.931(2) 1.000(3) 0.042 Uiso 1 1 d .
O5 O 0.97622(17) 0.61543(11) 0.98928(14) 0.0283(4) Uani 1 1 d .
N2 N 1.0688(2) 0.74686(14) 0.98418(18) 0.0278(5) Uani 1 1 d .
H2 H 1.068(3) 0.801(2) 0.978(2) 0.042 Uiso 1 1 d .
C10 C 0.7903(2) 0.82662(16) 0.98667(17) 0.0213(5) Uani 1 1 d .
C11 C 0.8191(2) 0.73501(15) 0.98320(17) 0.0212(5) Uani 1 1 d .
C12 C 0.7115(3) 0.67385(17) 0.97949(18) 0.0250(5) Uani 1 1 d .
H12 H 0.7301 0.6120 0.9777 0.030 Uiso 1 1 calc R
C13 C 0.5799(2) 0.70297(17) 0.97848(18) 0.0262(5) Uani 1 1 d .
H13 H 0.5076 0.6614 0.9765 0.031 Uiso 1 1 calc R
C14 C 0.5522(3) 0.79432(18) 0.98036(18) 0.0267(5) Uani 1 1 d .
H14 H 0.4610 0.8144 0.9793 0.032 Uiso 1 1 calc R
C15 C 0.6564(3) 0.85530(17) 0.98380(18) 0.0254(5) Uani 1 1 d .
H15 H 0.6367 0.9171 0.9842 0.030 Uiso 1 1 calc R
C16 C 0.9566(2) 0.70180(15) 0.98534(17) 0.0207(5) Uani 1 1 d .
C17 C 1.1233(3) 0.59770(17) 0.9891(2) 0.0284(6) Uani 1 1 d .
H17A H 1.1498 0.5639 0.9299 0.034 Uiso 1 1 calc R
H17B H 1.1504 0.5635 1.0479 0.034 Uiso 1 1 calc R
C18 C 1.1888(3) 0.68980(17) 0.9894(2) 0.0303(6) Uani 1 1 d .
H18A H 1.2412 0.7003 1.0502 0.036 Uiso 1 1 calc R
H18B H 1.2484 0.6984 0.9319 0.036 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'
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'
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 0.00 0.00 0.0630
-1.00 0.00 0.00 0.0360
0.00 -1.00 0.00 0.1470
0.00 1.00 0.00 0.1610
0.00 0.00 -1.00 0.0200
0.00 0.00 1.00 0.0250
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O1 Re1 O2 166.67(8)
O1 Re1 N1 89.72(8)
O2 Re1 N1 81.17(7)
O1 Re1 Cl3 97.94(6)
O2 Re1 Cl3 91.42(5)
N1 Re1 Cl3 87.59(6)
O1 Re1 Cl2 101.41(6)
O2 Re1 Cl2 88.16(5)
N1 Re1 Cl2 168.73(6)
Cl3 Re1 Cl2 89.08(2)
O1 Re1 Cl1 87.67(6)
O2 Re1 Cl1 82.83(5)
N1 Re1 Cl1 91.14(5)
Cl3 Re1 Cl1 174.24(2)
Cl2 Re1 Cl1 91.11(2)
C1 O2 Re1 133.06(15)
C7 O3 C8 107.30(17)
C7 N1 C9 109.26(19)
C7 N1 Re1 129.54(16)
C9 N1 Re1 121.01(14)
O2 C1 C6 118.8(2)
O2 C1 C2 121.9(2)
C6 C1 C2 119.3(2)
C3 C2 C1 119.7(2)
C3 C2 C7 121.5(2)
C1 C2 C7 118.8(2)
C4 C3 C2 120.4(2)
C4 C3 H3 119.8
C2 C3 H3 119.8
C3 C4 C5 119.9(2)
C3 C4 H4 120.0
C5 C4 H4 120.0
C6 C5 C4 120.8(2)
C6 C5 H5 119.6
C4 C5 H5 119.6
C5 C6 C1 119.9(2)
C5 C6 H6 120.0
C1 C6 H6 120.0
N1 C7 O3 115.9(2)
N1 C7 C2 126.4(2)
O3 C7 C2 117.69(19)
O3 C8 C9 104.55(17)
O3 C8 H8A 110.8
C9 C8 H8A 110.8
O3 C8 H8B 110.8
C9 C8 H8B 110.8
H8A C8 H8B 108.9
N1 C9 C8 102.78(18)
N1 C9 H9A 111.2
C8 C9 H9A 111.2
N1 C9 H9B 111.2
C8 C9 H9B 111.2
H9A C9 H9B 109.1
C10 O4 H4A 109(3)
C16 O5 C17 108.85(19)
C16 N2 C18 112.5(2)
C16 N2 H2 121(2)
C18 N2 H2 126(2)
O4 C10 C15 122.5(2)
O4 C10 C11 117.8(2)
C15 C10 C11 119.7(2)
C12 C11 C10 119.3(2)
C12 C11 C16 118.9(2)
C10 C11 C16 121.8(2)
C13 C12 C11 120.4(2)
C13 C12 H12 119.8
C11 C12 H12 119.8
C12 C13 C14 119.8(2)
C12 C13 H13 120.1
C14 C13 H13 120.1
C15 C14 C13 120.6(2)
C15 C14 H14 119.7
C13 C14 H14 119.7
C14 C15 C10 120.2(2)
C14 C15 H15 119.9
C10 C15 H15 119.9
N2 C16 O5 113.0(2)
N2 C16 C11 128.3(2)
O5 C16 C11 118.7(2)
O5 C17 C18 104.59(19)
O5 C17 H17A 110.8
C18 C17 H17A 110.8
O5 C17 H17B 110.8
C18 C17 H17B 110.8
H17A C17 H17B 108.9
N2 C18 C17 100.9(2)
N2 C18 H18A 111.6
C17 C18 H18A 111.6
N2 C18 H18B 111.6
C17 C18 H18B 111.6
H18A C18 H18B 109.4
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Re1 O1 1.6841(17)
Re1 O2 1.9778(16)
Re1 N1 2.0983(19)
Re1 Cl3 2.3621(7)
Re1 Cl2 2.3690(6)
Re1 Cl1 2.4701(6)
O2 C1 1.339(3)
O3 C7 1.349(3)
O3 C8 1.473(3)
N1 C7 1.292(3)
N1 C9 1.488(3)
C1 C6 1.404(3)
C1 C2 1.409(3)
C2 C3 1.400(3)
C2 C7 1.453(3)
C3 C4 1.381(4)
C3 H3 0.9500
C4 C5 1.392(4)
C4 H4 0.9500
C5 C6 1.383(4)
C5 H5 0.9500
C6 H6 0.9500
C8 C9 1.536(3)
C8 H8A 0.9900
C8 H8B 0.9900
C9 H9A 0.9900
C9 H9B 0.9900
O4 C10 1.354(3)
O4 H4A 0.77(3)
O5 C16 1.316(3)
O5 C17 1.477(3)
N2 C16 1.299(3)
N2 C18 1.465(3)
N2 H2 0.82(3)
C10 C15 1.391(3)
C10 C11 1.409(3)
C11 C12 1.407(3)
C11 C16 1.448(3)
C12 C13 1.371(4)
C12 H12 0.9500
C13 C14 1.402(4)
C13 H13 0.9500
C14 C15 1.379(4)
C14 H14 0.9500
C15 H15 0.9500
C17 C18 1.530(4)
C17 H17A 0.9900
C17 H17B 0.9900
C18 H18A 0.9900
C18 H18B 0.9900
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
O4 H4A Cl1 0.77(3) 2.39(3) 3.1470(19) 167(4) 1_566
N2 H2 O4 0.82(3) 2.12(3) 2.677(3) 126(3) .
N2 H2 Cl1 0.82(3) 2.52(3) 3.206(2) 142(3) 3_766
