#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:32:08 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179065 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/27/4302750.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_4302750
loop_
_publ_author_name
'Zhaoqing Xu'
'Ming-Dong Zhou'
'Markus Drees'
'Hugh Chaffey-Millar'
'Eberhardt Herdtweck'
'Wolfgang A. Herrmann'
'Fritz E. Kühn'
_publ_contact_author_address
;
       Department Chemie,
       Lehrstuhl für Anorganische Chemie,
       Technische Universität München,
       Lichtenbergstrasse 4,
       D-85747 Garching bei München,
       Germany.
;
_publ_contact_author_email       eberhardt.herdtweck@ch.tum.de
_publ_contact_author_fax         '+49(0)89 289 13473'
_publ_contact_author_name
;
       Dr. Eberhardt Herdtweck
;
_publ_contact_author_phone       '+49(0)89 289 13143'
_publ_section_title
;
Mono- and Bis- Methyltrioxorhenium(VII) Complexes with Salen Ligands:
Synthesis, Properties, Applications
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6812
_journal_page_last               6822
_journal_paper_doi               10.1021/ic900761u
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C22 H26 Br2 N2 O8 Re2'
_chemical_formula_sum            'C22 H26 Br2 N2 O8 Re2'
_chemical_formula_weight         978.67
_chemical_name_systematic        ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 116.257(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.6278(13)
_cell_length_b                   8.7700(2)
_cell_length_c                   24.9535(12)
_cell_measurement_reflns_used    28669
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      27.24
_cell_measurement_theta_min      2.47
_cell_volume                     5422.3(4)
_computing_cell_refinement       'X-AREA (Stoe, 2004)'
_computing_data_collection       'X-AREA (Stoe, 2004)'
_computing_data_reduction        'X-AREA (Stoe, 2004)'
_computing_molecular_graphics    'PLATON (Spek, 2007)'
_computing_publication_material  'PLATON (Spek, 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1998)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      173(1)
_diffrn_detector                 'image plate'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'IPDS 2T (Stoe)'
_diffrn_measurement_method       'omega-rotation/oscillation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'NONIUS FR 591 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.059
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            34454
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         4.69
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    11.916
_exptl_absorpt_correction_T_max  0.5746
_exptl_absorpt_correction_T_min  0.0364
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 Numerical absorption correction after crystal shape optimization
 source: (Stoe, 2004)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.398
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4893
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0189
_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)+(0.0261P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0406
_refine_ls_wR_factor_ref         0.0418
_reflns_number_gt                4148
_reflns_number_total             4893
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic900761u_si_002_3.cif
_cod_data_source_block           Compound_7
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4302750
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,y,1/2-z
3 -x,-y,-z
4 x,-y,1/2+z
5 1/2+x,1/2+y,z
6 1/2-x,1/2+y,1/2-z
7 1/2-x,1/2-y,-z
8 1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
Re1 Re Uani 0.10715(1) 0.47701(2) -0.03731(1) 1.000 0.0220(1) . .
Re2 Re Uani 0.18262(1) 1.11045(2) 0.14663(1) 1.000 0.0198(1) . .
Br1 Br Uani 0.41135(2) 0.55583(8) 0.17784(2) 1.000 0.0466(2) . .
Br2 Br Uani -0.04020(2) 0.89750(5) -0.16795(2) 1.000 0.0273(1) . .
O1 O Uani 0.14158(13) 0.3227(4) -0.04475(15) 1.000 0.0320(10) . .
O2 O Uani 0.06848(12) 0.4559(3) 0.00071(15) 1.000 0.0293(10) . .
O3 O Uani 0.06040(16) 0.5133(5) -0.10837(16) 1.000 0.0519(14) . .
O4 O Uani 0.16955(11) 0.4859(4) 0.05498(13) 1.000 0.0265(9) . .
O5 O Uani 0.18425(13) 0.9802(3) 0.19869(13) 1.000 0.0294(10) . .
O6 O Uani 0.13065(12) 1.2404(3) 0.11855(14) 1.000 0.0282(9) . .
O7 O Uani 0.23821(13) 1.2206(4) 0.18660(14) 1.000 0.0325(10) . .
O8 O Uani 0.12178(12) 0.9498(3) 0.09000(13) 1.000 0.0241(9) . .
N1 N Uani 0.17031(13) 0.5507(4) 0.15947(15) 1.000 0.0179(10) . .
N2 N Uani 0.07719(13) 0.7254(4) 0.11522(15) 1.000 0.0186(10) . .
C1 C Uani 0.1439(2) 0.6902(5) -0.0363(3) 1.000 0.0394(16) . .
C2 C Uani 0.2175(2) 1.0438(6) 0.0895(2) 1.000 0.0329(17) . .
C3 C Uani 0.22233(16) 0.5005(5) 0.08006(19) 1.000 0.0212(12) . .
C4 C Uani 0.25496(17) 0.4655(5) 0.0514(2) 1.000 0.0255(12) . .
C5 C Uani 0.31004(17) 0.4803(5) 0.08021(19) 1.000 0.0248(12) . .
C6 C Uani 0.33518(16) 0.5339(5) 0.13924(19) 1.000 0.0247(12) . .
C7 C Uani 0.30582(17) 0.5696(5) 0.16903(19) 1.000 0.0260(12) . .
C8 C Uani 0.24895(16) 0.5527(5) 0.14028(18) 1.000 0.0193(12) . .
C9 C Uani 0.22044(17) 0.5826(5) 0.17526(19) 1.000 0.0213(12) . .
C10 C Uani 0.14391(16) 0.5832(4) 0.19812(17) 1.000 0.0165(11) . .
C11 C Uani 0.15308(18) 0.4559(5) 0.2441(2) 1.000 0.0239(12) . .
C12 C Uani 0.12816(19) 0.5028(5) 0.2851(2) 1.000 0.0281(12) . .
C13 C Uani 0.06784(19) 0.5385(6) 0.2492(2) 1.000 0.0301(14) . .
C14 C Uani 0.05816(17) 0.6591(5) 0.2009(2) 1.000 0.0237(12) . .
C15 C Uani 0.08338(16) 0.6095(5) 0.16008(18) 1.000 0.0186(11) . .
C16 C Uani 0.04469(16) 0.7191(5) 0.05850(18) 1.000 0.0190(11) . .
C17 C Uani 0.04551(16) 0.8284(5) 0.01647(18) 1.000 0.0182(11) . .
C18 C Uani 0.00698(16) 0.8147(5) -0.04440(19) 1.000 0.0210(11) . .
C19 C Uani 0.00842(16) 0.9170(5) -0.08529(18) 1.000 0.0196(11) . .
C20 C Uani 0.04560(17) 1.0357(5) -0.06829(19) 1.000 0.0211(12) . .
C21 C Uani 0.08349(17) 1.0510(5) -0.00959(19) 1.000 0.0201(11) . .
C22 C Uani 0.08477(16) 0.9470(5) 0.03412(18) 1.000 0.0186(11) . .
H1 H Uiso 0.15130 0.50800 0.12440 1.000 0.0210 calc R
H2 H Uiso 0.09750 0.80730 0.12790 1.000 0.0220 calc R
H11 H Uiso 0.15700 0.73580 0.00350 1.000 0.0590 calc R
H12 H Uiso 0.11730 0.75830 -0.06590 1.000 0.0590 calc R
H13 H Uiso 0.17420 0.67490 -0.04610 1.000 0.0590 calc R
H17 H Uiso 0.32330 0.60590 0.20900 1.000 0.0310 calc R
H21 H Uiso 0.19480 0.96610 0.06140 1.000 0.0500 calc R
H22 H Uiso 0.25360 1.00180 0.11350 1.000 0.0500 calc R
H23 H Uiso 0.22020 1.13270 0.06720 1.000 0.0500 calc R
H41 H Uiso 0.23840 0.43100 0.01110 1.000 0.0300 calc R
H51 H Uiso 0.33120 0.45420 0.06020 1.000 0.0300 calc R
H91 H Uiso 0.24000 0.62980 0.21310 1.000 0.0260 calc R
H101 H Uiso 0.15980 0.67940 0.22050 1.000 0.0200 calc R
H111 H Uiso 0.13630 0.36000 0.22320 1.000 0.0280 calc R
H112 H Uiso 0.19230 0.43800 0.26790 1.000 0.0280 calc R
H116 H Uiso 0.01930 0.63820 0.04430 1.000 0.0230 calc R
H121 H Uiso 0.14710 0.59410 0.30820 1.000 0.0340 calc R
H122 H Uiso 0.13280 0.41940 0.31370 1.000 0.0340 calc R
H131 H Uiso 0.04830 0.44390 0.23000 1.000 0.0360 calc R
H132 H Uiso 0.05330 0.57580 0.27660 1.000 0.0360 calc R
H141 H Uiso 0.01890 0.67450 0.17680 1.000 0.0290 calc R
H142 H Uiso 0.07410 0.75740 0.22020 1.000 0.0290 calc R
H151 H Uiso 0.06620 0.51230 0.13950 1.000 0.0230 calc R
H181 H Uiso -0.01940 0.73600 -0.05660 1.000 0.0250 calc R
H201 H Uiso 0.04490 1.10690 -0.09730 1.000 0.0250 calc R
H211 H Uiso 0.10890 1.13210 0.00150 1.000 0.0240 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Re Re -1.0185 7.2310 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
C C 0.0033 0.0016 '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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Re1 O2 118.97(15) . . . yes
O1 Re1 O3 103.73(19) . . . yes
O1 Re1 O4 85.71(15) . . . yes
O1 Re1 C1 114.3(2) . . . yes
O2 Re1 O3 103.0(2) . . . yes
O2 Re1 O4 79.39(14) . . . yes
O2 Re1 C1 119.85(19) . . . yes
O3 Re1 O4 167.11(17) . . . yes
O3 Re1 C1 89.2(2) . . . yes
O4 Re1 C1 78.8(2) . . . yes
O5 Re2 O6 119.14(17) . . . yes
O5 Re2 O7 102.61(15) . . . yes
O5 Re2 O8 79.28(13) . . . yes
O5 Re2 C2 117.19(18) . . . yes
O6 Re2 O7 103.61(16) . . . yes
O6 Re2 O8 84.17(13) . . . yes
O6 Re2 C2 116.95(17) . . . yes
O7 Re2 O8 169.36(15) . . . yes
O7 Re2 C2 89.42(19) . . . yes
O8 Re2 C2 80.51(17) . . . yes
Re1 O4 C3 134.2(3) . . . yes
Re2 O8 C22 135.9(3) . . . yes
C9 N1 C10 122.2(4) . . . yes
C15 N2 C16 126.4(4) . . . yes
C10 N1 H1 119.00 . . . no
C9 N1 H1 119.00 . . . no
C16 N2 H2 117.00 . . . no
C15 N2 H2 117.00 . . . no
O4 C3 C4 124.1(4) . . . yes
C4 C3 C8 117.2(4) . . . no
O4 C3 C8 118.7(4) . . . yes
C3 C4 C5 121.6(4) . . . no
C4 C5 C6 120.1(4) . . . no
C5 C6 C7 120.9(4) . . . no
Br1 C6 C5 119.3(4) . . . yes
Br1 C6 C7 119.7(3) . . . yes
C6 C7 C8 119.7(4) . . . no
C3 C8 C9 122.3(4) . . . no
C7 C8 C9 117.2(4) . . . no
C3 C8 C7 120.5(4) . . . no
N1 C9 C8 125.3(4) . . . yes
N1 C10 C11 112.5(3) . . . yes
N1 C10 C15 110.2(3) . . . yes
C11 C10 C15 110.2(4) . . . no
C10 C11 C12 109.3(4) . . . no
C11 C12 C13 111.1(4) . . . no
C12 C13 C14 111.5(4) . . . no
C13 C14 C15 110.8(4) . . . no
N2 C15 C10 107.7(4) . . . yes
N2 C15 C14 112.2(4) . . . yes
C10 C15 C14 108.9(3) . . . no
N2 C16 C17 122.9(4) . . . yes
C16 C17 C22 121.3(4) . . . no
C18 C17 C22 120.0(4) . . . no
C16 C17 C18 118.7(4) . . . no
C17 C18 C19 119.0(4) . . . no
Br2 C19 C18 120.5(3) . . . yes
Br2 C19 C20 118.0(3) . . . yes
C18 C19 C20 121.5(4) . . . no
C19 C20 C21 120.5(4) . . . no
C20 C21 C22 120.4(4) . . . no
O8 C22 C21 123.4(4) . . . yes
C17 C22 C21 118.6(4) . . . no
O8 C22 C17 118.0(4) . . . yes
Re1 C1 H11 109.00 . . . no
Re1 C1 H12 109.00 . . . no
Re1 C1 H13 109.00 . . . no
H11 C1 H12 109.00 . . . no
H11 C1 H13 110.00 . . . no
H12 C1 H13 109.00 . . . no
Re2 C2 H21 110.00 . . . no
Re2 C2 H22 110.00 . . . no
Re2 C2 H23 109.00 . . . no
H21 C2 H22 109.00 . . . no
H21 C2 H23 109.00 . . . no
H22 C2 H23 109.00 . . . no
C3 C4 H41 119.00 . . . no
C5 C4 H41 119.00 . . . no
C4 C5 H51 120.00 . . . no
C6 C5 H51 120.00 . . . no
C6 C7 H17 120.00 . . . no
C8 C7 H17 120.00 . . . no
N1 C9 H91 117.00 . . . no
C8 C9 H91 117.00 . . . no
N1 C10 H101 108.00 . . . no
C11 C10 H101 108.00 . . . no
C15 C10 H101 108.00 . . . no
C10 C11 H111 110.00 . . . no
C10 C11 H112 110.00 . . . no
C12 C11 H111 110.00 . . . no
C12 C11 H112 110.00 . . . no
H111 C11 H112 108.00 . . . no
C11 C12 H121 109.00 . . . no
C11 C12 H122 109.00 . . . no
C13 C12 H121 109.00 . . . no
C13 C12 H122 109.00 . . . no
H121 C12 H122 108.00 . . . no
C12 C13 H131 109.00 . . . no
C12 C13 H132 109.00 . . . no
C14 C13 H131 109.00 . . . no
C14 C13 H132 109.00 . . . no
H131 C13 H132 108.00 . . . no
C13 C14 H141 110.00 . . . no
C13 C14 H142 109.00 . . . no
C15 C14 H141 110.00 . . . no
C15 C14 H142 110.00 . . . no
H141 C14 H142 108.00 . . . no
N2 C15 H151 109.00 . . . no
C10 C15 H151 109.00 . . . no
C14 C15 H151 109.00 . . . no
N2 C16 H116 119.00 . . . no
C17 C16 H116 118.00 . . . no
C17 C18 H181 121.00 . . . no
C19 C18 H181 120.00 . . . no
C19 C20 H201 120.00 . . . no
C21 C20 H201 120.00 . . . no
C20 C21 H211 120.00 . . . no
C22 C21 H211 120.00 . . . no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 O1 1.711(4) . . yes
Re1 O2 1.724(4) . . yes
Re1 O3 1.699(4) . . yes
Re1 O4 2.184(3) . . yes
Re1 C1 2.122(5) . . yes
Re2 O5 1.715(3) . . yes
Re2 O6 1.721(3) . . yes
Re2 O7 1.712(4) . . yes
Re2 O8 2.169(3) . . yes
Re2 C2 2.126(5) . . yes
Br1 C6 1.897(5) . . yes
Br2 C19 1.907(4) . . yes
O4 C3 1.314(6) . . yes
O8 C22 1.315(5) . . yes
N1 C9 1.292(6) . . yes
N1 C10 1.472(6) . . yes
N2 C15 1.465(5) . . yes
N2 C16 1.299(5) . . yes
N1 H1 0.8800 . . no
N2 H2 0.8800 . . no
C3 C8 1.425(6) . . no
C3 C4 1.410(7) . . no
C4 C5 1.372(7) . . no
C5 C6 1.403(6) . . no
C6 C7 1.357(7) . . no
C7 C8 1.417(7) . . no
C8 C9 1.435(7) . . no
C10 C15 1.532(6) . . no
C10 C11 1.539(6) . . no
C11 C12 1.521(7) . . no
C12 C13 1.535(8) . . no
C13 C14 1.536(7) . . no
C14 C15 1.530(7) . . no
C16 C17 1.428(6) . . no
C17 C22 1.425(6) . . no
C17 C18 1.423(6) . . no
C18 C19 1.372(6) . . no
C19 C20 1.390(7) . . no
C20 C21 1.379(6) . . no
C21 C22 1.410(6) . . no
C1 H11 0.9800 . . no
C1 H12 0.9800 . . no
C1 H13 0.9800 . . no
C2 H21 0.9800 . . no
C2 H22 0.9800 . . no
C2 H23 0.9800 . . no
C4 H41 0.9500 . . no
C5 H51 0.9500 . . no
C7 H17 0.9500 . . no
C9 H91 0.9500 . . no
C10 H101 1.0000 . . no
C11 H111 0.9900 . . no
C11 H112 0.9900 . . no
C12 H121 0.9900 . . no
C12 H122 0.9900 . . no
C13 H131 0.9900 . . no
C13 H132 0.9900 . . no
C14 H141 0.9900 . . no
C14 H142 0.9900 . . no
C15 H151 1.0000 . . no
C16 H116 0.9500 . . no
C18 H181 0.9500 . . no
C20 H201 0.9500 . . no
C21 H211 0.9500 . . no
