#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:48:26 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179348 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/45/4324565.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_4324565
loop_
_publ_author_name
'Pedro Traar'
'Jörg A. Schachner'
'Lisa Steiner'
'Anna Sachse'
'Manuel Volpe'
'Nadia C. Mösch-Zanetti'
_publ_section_title
;
 Oxorhenium(V) Complexes with Pyrazole Based Aryloxide Ligands and
 Application in Olefin Epoxidation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1983
_journal_page_last               1990
_journal_paper_doi               10.1021/ic102455v
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C32 H26 Br2 N2 O2 P Re'
_chemical_formula_sum            'C32 H26 Br2 N2 O2 P Re'
_chemical_formula_weight         847.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 109.515(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0730(7)
_cell_length_b                   12.8745(6)
_cell_length_c                   15.3274(7)
_cell_measurement_reflns_used    9177
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.3
_cell_measurement_theta_min      2.70
_cell_volume                     2803.5(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Giacovazzo, 1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            184234
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         37.23
_diffrn_reflns_theta_min         2.12
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.276
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.5854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.008
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.737
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         14516
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0241
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0166P)²+3.7452P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0438
_refine_ls_wR_factor_ref         0.0489
_reflns_number_gt                11421
_reflns_number_total             14516
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102455v_si_002_8.cif
_cod_data_source_block           remebr
_cod_database_code               4324565
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 0.765137(4) 0.039043(5) 0.098538(4) 0.00845(2) Uani 1 1 d .
Br1 Br 0.771280(13) -0.000332(15) -0.063201(12) 0.01395(3) Uani 1 1 d .
Br2 Br 0.644038(13) -0.100299(14) 0.075625(13) 0.01482(4) Uani 1 1 d .
P1 P 0.75709(3) 0.08148(3) 0.25352(3) 0.00854(7) Uani 1 1 d .
N1 N 0.85085(10) 0.17371(12) 0.09831(10) 0.0101(2) Uani 1 1 d .
N2 N 0.93653(10) 0.17048(12) 0.08637(11) 0.0125(3) Uani 1 1 d .
O1 O 0.86251(9) -0.02699(10) 0.16241(9) 0.0123(2) Uani 1 1 d .
O2 O 0.66798(9) 0.14168(10) 0.04656(9) 0.0107(2) Uani 1 1 d .
C1 C 0.65550(12) 0.24238(13) 0.06180(12) 0.0102(3) Uani 1 1 d .
C2 C 0.56295(12) 0.27770(15) 0.04746(13) 0.0134(3) Uani 1 1 d .
H2 H 0.5109 0.2325 0.0217 0.016 Uiso 1 1 calc R
C3 C 0.54877(12) 0.37665(15) 0.07073(13) 0.0135(3) Uani 1 1 d .
H3 H 0.4864 0.4002 0.0606 0.016 Uiso 1 1 calc R
C4 C 0.62513(12) 0.44548(14) 0.10986(12) 0.0117(3) Uani 1 1 d .
C5 C 0.71855(12) 0.41226(13) 0.12023(12) 0.0103(3) Uani 1 1 d .
C6 C 0.73216(12) 0.30908(13) 0.09105(12) 0.0098(3) Uani 1 1 d .
C7 C 0.82305(12) 0.27423(14) 0.08700(12) 0.0103(3) Uani 1 1 d .
C8 C 0.89149(13) 0.33403(15) 0.06651(13) 0.0143(3) Uani 1 1 d .
H8 H 0.8894 0.4065 0.0542 0.017 Uiso 1 1 calc R
C9 C 0.96201(13) 0.26582(15) 0.06804(14) 0.0157(3) Uani 1 1 d .
H9 H 1.0191 0.2831 0.0579 0.019 Uiso 1 1 calc R
C10 C 0.99528(13) 0.07876(15) 0.10200(15) 0.0169(3) Uani 1 1 d .
H10A H 1.0513 0.0933 0.0851 0.025 Uiso 1 1 calc R
H10B H 0.9598 0.0215 0.0640 0.025 Uiso 1 1 calc R
H10C H 1.0145 0.0593 0.1675 0.025 Uiso 1 1 calc R
C11 C 0.61010(13) 0.54614(15) 0.13920(13) 0.0141(3) Uani 1 1 d .
H11 H 0.5478 0.5679 0.1317 0.017 Uiso 1 1 calc R
C12 C 0.68318(13) 0.61261(15) 0.17805(13) 0.0155(3) Uani 1 1 d .
H12 H 0.6717 0.6807 0.1956 0.019 Uiso 1 1 calc R
C13 C 0.77582(13) 0.57902(15) 0.19184(13) 0.0147(3) Uani 1 1 d .
H13 H 0.8270 0.6244 0.2205 0.018 Uiso 1 1 calc R
C14 C 0.79330(12) 0.48182(14) 0.16452(12) 0.0123(3) Uani 1 1 d .
H14 H 0.8565 0.4606 0.1754 0.015 Uiso 1 1 calc R
C15 C 0.86699(12) 0.14640(13) 0.31644(12) 0.0102(3) Uani 1 1 d .
C16 C 0.87909(13) 0.25244(14) 0.30468(13) 0.0138(3) Uani 1 1 d .
H16 H 0.8260 0.2944 0.2737 0.017 Uiso 1 1 calc R
C17 C 0.96793(14) 0.29714(15) 0.33778(14) 0.0169(3) Uani 1 1 d .
H17 H 0.9751 0.3694 0.3295 0.020 Uiso 1 1 calc R
C18 C 1.04629(13) 0.23702(16) 0.38295(14) 0.0179(4) Uani 1 1 d .
H18 H 1.1072 0.2674 0.4040 0.021 Uiso 1 1 calc R
C19 C 1.03472(13) 0.13186(16) 0.39702(14) 0.0175(4) Uani 1 1 d .
H19 H 1.0878 0.0907 0.4295 0.021 Uiso 1 1 calc R
C20 C 0.94601(13) 0.08658(15) 0.36380(13) 0.0139(3) Uani 1 1 d .
H20 H 0.9389 0.0146 0.3733 0.017 Uiso 1 1 calc R
C21 C 0.75299(12) -0.03158(13) 0.32375(12) 0.0103(3) Uani 1 1 d .
C22 C 0.78538(12) -0.12938(14) 0.30844(12) 0.0125(3) Uani 1 1 d .
H22 H 0.8123 -0.1382 0.2611 0.015 Uiso 1 1 calc R
C23 C 0.77825(13) -0.21395(15) 0.36248(13) 0.0139(3) Uani 1 1 d .
H23 H 0.8010 -0.2800 0.3520 0.017 Uiso 1 1 calc R
C24 C 0.73826(12) -0.20254(15) 0.43143(13) 0.0138(3) Uani 1 1 d .
H24 H 0.7316 -0.2609 0.4667 0.017 Uiso 1 1 calc R
C25 C 0.70805(12) -0.10519(15) 0.44840(13) 0.0139(3) Uani 1 1 d .
H25 H 0.6825 -0.0966 0.4968 0.017 Uiso 1 1 calc R
C26 C 0.71483(12) -0.02028(15) 0.39520(12) 0.0124(3) Uani 1 1 d .
H26 H 0.6935 0.0459 0.4072 0.015 Uiso 1 1 calc R
C27 C 0.65733(12) 0.15794(14) 0.25779(12) 0.0106(3) Uani 1 1 d .
C28 C 0.56827(12) 0.11951(15) 0.20552(13) 0.0135(3) Uani 1 1 d .
H28 H 0.5631 0.0591 0.1686 0.016 Uiso 1 1 calc R
C29 C 0.48767(13) 0.17004(16) 0.20795(14) 0.0161(3) Uani 1 1 d .
H29 H 0.4273 0.1438 0.1731 0.019 Uiso 1 1 calc R
C30 C 0.49519(13) 0.25915(16) 0.26145(14) 0.0167(3) Uani 1 1 d .
H30 H 0.4401 0.2947 0.2617 0.020 Uiso 1 1 calc R
C31 C 0.58314(14) 0.29597(16) 0.31429(14) 0.0172(3) Uani 1 1 d .
H31 H 0.5880 0.3560 0.3517 0.021 Uiso 1 1 calc R
C32 C 0.66449(13) 0.24554(15) 0.31299(13) 0.0144(3) Uani 1 1 d .
H32 H 0.7246 0.2708 0.3496 0.017 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
Re Re -1.0185 7.2310 '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'
P P 0.1023 0.0942 '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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O1 Re1 O2 165.91(6)
O1 Re1 N1 90.03(6)
O2 Re1 N1 79.77(5)
O1 Re1 P1 82.38(4)
O2 Re1 P1 88.37(4)
N1 Re1 P1 92.60(4)
O1 Re1 Br2 99.90(4)
O2 Re1 Br2 90.89(4)
N1 Re1 Br2 169.69(4)
P1 Re1 Br2 91.468(11)
O1 Re1 Br1 98.93(4)
O2 Re1 Br1 90.21(4)
N1 Re1 Br1 86.69(4)
P1 Re1 Br1 178.507(12)
Br2 Re1 Br1 89.013(7)
C27 P1 C15 110.50(8)
C27 P1 C21 102.68(8)
C15 P1 C21 104.97(8)
C27 P1 Re1 117.38(6)
C15 P1 Re1 106.38(6)
C21 P1 Re1 114.32(6)
C7 N1 N2 106.17(14)
C7 N1 Re1 127.38(11)
N2 N1 Re1 124.65(11)
C9 N2 N1 110.47(15)
C9 N2 C10 125.33(15)
N1 N2 C10 123.85(15)
C1 O2 Re1 135.96(11)
O2 C1 C6 120.26(15)
O2 C1 C2 118.20(15)
C6 C1 C2 121.55(16)
C3 C2 C1 119.64(17)
C2 C3 C4 121.37(16)
C11 C4 C3 120.91(16)
C11 C4 C5 119.70(16)
C3 C4 C5 119.39(16)
C14 C5 C4 117.32(16)
C14 C5 C6 123.90(15)
C4 C5 C6 118.66(15)
C1 C6 C5 118.81(15)
C1 C6 C7 119.14(15)
C5 C6 C7 121.98(15)
N1 C7 C8 109.50(15)
N1 C7 C6 122.83(15)
C8 C7 C6 127.58(16)
C9 C8 C7 105.54(16)
N2 C9 C8 108.31(16)
C12 C11 C4 121.44(17)
C11 C12 C13 119.22(17)
C14 C13 C12 121.04(18)
C13 C14 C5 121.18(16)
C16 C15 C20 118.64(16)
C16 C15 P1 121.06(13)
C20 C15 P1 119.25(13)
C17 C16 C15 120.63(17)
C18 C17 C16 120.47(18)
C17 C18 C19 119.35(18)
C20 C19 C18 120.42(18)
C19 C20 C15 120.45(17)
C22 C21 C26 118.75(16)
C22 C21 P1 122.49(13)
C26 C21 P1 118.76(13)
C23 C22 C21 120.21(16)
C24 C23 C22 120.60(17)
C25 C24 C23 119.44(17)
C24 C25 C26 120.54(17)
C25 C26 C21 120.42(17)
C32 C27 C28 119.84(16)
C32 C27 P1 124.32(13)
C28 C27 P1 115.71(13)
C29 C28 C27 119.85(17)
C28 C29 C30 120.10(18)
C31 C30 C29 119.99(17)
C30 C31 C32 120.45(18)
C27 C32 C31 119.75(17)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Re1 O1 1.6957(13)
Re1 O2 1.9354(12)
Re1 N1 2.1630(15)
Re1 P1 2.4796(4)
Re1 Br2 2.4990(2)
Re1 Br1 2.5621(2)
P1 C27 1.8166(17)
P1 C15 1.8181(17)
P1 C21 1.8236(18)
N1 C7 1.353(2)
N1 N2 1.364(2)
N2 C9 1.344(2)
N2 C10 1.447(2)
O2 C1 1.342(2)
C1 C6 1.388(2)
C1 C2 1.413(2)
C2 C3 1.359(3)
C3 C4 1.417(3)
C4 C11 1.415(3)
C4 C5 1.429(2)
C5 C14 1.422(2)
C5 C6 1.438(2)
C6 C7 1.463(2)
C7 C8 1.404(2)
C8 C9 1.373(3)
C11 C12 1.365(3)
C12 C13 1.409(3)
C13 C14 1.373(3)
C15 C16 1.397(3)
C15 C20 1.400(2)
C16 C17 1.388(3)
C17 C18 1.388(3)
C18 C19 1.391(3)
C19 C20 1.390(3)
C21 C22 1.398(2)
C21 C26 1.404(2)
C22 C23 1.394(3)
C23 C24 1.388(3)
C24 C25 1.387(3)
C25 C26 1.388(3)
C27 C32 1.392(3)
C27 C28 1.404(2)
C28 C29 1.390(3)
C29 C30 1.393(3)
C30 C31 1.386(3)
C31 C32 1.393(3)
