#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/45/4324564.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_4324564
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
'C28 H26 Cl N4 O3 Re, C H Cl3, 0.5 (C4 H10 O)'
_chemical_formula_sum            'C31 H28 Cl4 N4 O3.5 Re'
_chemical_formula_weight         840.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.172(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.108(4)
_cell_length_b                   12.7947(16)
_cell_length_c                   15.1945(19)
_cell_measurement_reflns_used    9477
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.01
_cell_measurement_theta_min      2.46
_cell_volume                     6335.3(14)
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0466
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            96602
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         31.08
_diffrn_reflns_theta_min         2.09
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.215
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.5409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3304
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.905
_refine_diff_density_min         -3.383
_refine_diff_density_rms         0.351
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         9892
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1431P)²+23.4200P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1759
_refine_ls_wR_factor_ref         0.1963
_reflns_number_gt                8101
_reflns_number_total             9892
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102455v_si_002_7.cif
_cod_data_source_block           renacl2
_cod_original_cell_volume        6335.4(14)
_cod_original_formula_sum        'C31 H28 Cl4 N4 O3.50 Re'
_cod_database_code               4324564
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.772253(6) 0.508569(16) 0.842582(12) 0.01429(10) Uani 1 1 d . . .
Cl1 Cl 0.73902(4) 0.45905(10) 0.95281(8) 0.0207(3) Uani 1 1 d . . .
O1 O 0.73264(17) 0.5116(3) 0.7452(3) 0.0244(10) Uani 1 1 d . . .
O2 O 0.78959(12) 0.3606(3) 0.8514(2) 0.0190(7) Uani 1 1 d . . .
O3 O 0.82579(12) 0.5334(3) 0.9394(2) 0.0158(7) Uani 1 1 d . . .
N1 N 0.81105(15) 0.5321(4) 0.7564(3) 0.0176(8) Uani 1 1 d . . .
N2 N 0.80414(14) 0.5953(3) 0.6812(3) 0.0182(8) Uani 1 1 d . . .
N3 N 0.76675(13) 0.6695(3) 0.8691(3) 0.0145(8) Uani 1 1 d . . .
N4 N 0.73208(13) 0.7228(3) 0.8718(3) 0.0167(8) Uani 1 1 d . . .
C1 C 0.82781(17) 0.3288(4) 0.8575(3) 0.0176(10) Uani 1 1 d . . .
C2 C 0.84061(18) 0.2357(4) 0.9111(3) 0.0225(11) Uani 1 1 d . . .
H2 H 0.8222 0.2015 0.9378 0.027 Uiso 1 1 calc R . .
C3 C 0.87885(19) 0.1961(4) 0.9238(4) 0.0245(11) Uani 1 1 d . . .
H3 H 0.8861 0.1324 0.9566 0.029 Uiso 1 1 calc R . .
C4 C 0.90846(17) 0.2478(4) 0.8893(3) 0.0204(10) Uani 1 1 d . . .
C5 C 0.89640(17) 0.3412(4) 0.8380(3) 0.0189(10) Uani 1 1 d . . .
C6 C 0.85529(15) 0.3784(4) 0.8179(3) 0.0153(9) Uani 1 1 d . . .
C7 C 0.84038(17) 0.4618(4) 0.7508(3) 0.0167(9) Uani 1 1 d . . .
C8 C 0.8521(2) 0.4842(4) 0.6715(4) 0.0210(11) Uani 1 1 d . . .
H8 H 0.8722 0.4487 0.6508 0.025 Uiso 1 1 calc R . .
C9 C 0.82842(18) 0.5685(5) 0.6298(3) 0.0222(11) Uani 1 1 d . . .
H9 H 0.8292 0.6016 0.5744 0.027 Uiso 1 1 calc R . .
C10 C 0.77594(18) 0.6841(5) 0.6647(3) 0.0237(11) Uani 1 1 d . . .
H10A H 0.7734 0.7137 0.6038 0.036 Uiso 1 1 calc R . .
H10B H 0.7866 0.7375 0.7120 0.036 Uiso 1 1 calc R . .
H10C H 0.7490 0.6607 0.6674 0.036 Uiso 1 1 calc R . .
C11 C 0.94892(19) 0.2100(5) 0.9094(4) 0.0260(12) Uani 1 1 d . . .
H11 H 0.9562 0.1465 0.9427 0.031 Uiso 1 1 calc R . .
C12 C 0.9780(2) 0.2641(6) 0.8813(4) 0.0320(14) Uani 1 1 d . . .
H12 H 1.0049 0.2365 0.8925 0.038 Uiso 1 1 calc R . .
C13 C 0.96771(19) 0.3600(5) 0.8362(4) 0.0287(12) Uani 1 1 d . . .
H13 H 0.9882 0.3997 0.8205 0.034 Uiso 1 1 calc R . .
C14 C 0.92791(17) 0.3977(5) 0.8141(3) 0.0235(11) Uani 1 1 d . . .
H14 H 0.9215 0.4624 0.7824 0.028 Uiso 1 1 calc R . .
C15 C 0.85331(16) 0.6076(4) 0.9364(3) 0.0160(9) Uani 1 1 d . . .
C16 C 0.89537(17) 0.5794(4) 0.9635(3) 0.0211(10) Uani 1 1 d . . .
H16 H 0.9034 0.5117 0.9880 0.025 Uiso 1 1 calc R . .
C17 C 0.92434(17) 0.6483(4) 0.9548(3) 0.0215(10) Uani 1 1 d . . .
H17 H 0.9525 0.6288 0.9740 0.026 Uiso 1 1 calc R . .
C18 C 0.91266(16) 0.7499(4) 0.9169(3) 0.0176(10) Uani 1 1 d . . .
C19 C 0.87071(17) 0.7809(4) 0.8931(3) 0.0168(9) Uani 1 1 d . . .
C20 C 0.84121(17) 0.7084(4) 0.9079(3) 0.0166(9) Uani 1 1 d . . .
C21 C 0.79826(16) 0.7396(4) 0.8963(3) 0.0171(9) Uani 1 1 d . . .
C22 C 0.78326(17) 0.8349(4) 0.9170(3) 0.0194(10) Uani 1 1 d . . .
H22 H 0.7986 0.8966 0.9385 0.023 Uiso 1 1 calc R . .
C23 C 0.74129(17) 0.8209(4) 0.8997(3) 0.0193(10) Uani 1 1 d . . .
H23 H 0.7224 0.8725 0.9066 0.023 Uiso 1 1 calc R . .
C24 C 0.69115(16) 0.6764(4) 0.8408(3) 0.0201(10) Uani 1 1 d . . .
H24A H 0.6712 0.7245 0.8537 0.030 Uiso 1 1 calc R . .
H24B H 0.6910 0.6103 0.8734 0.030 Uiso 1 1 calc R . .
H24C H 0.6838 0.6631 0.7744 0.030 Uiso 1 1 calc R . .
C25 C 0.94250(19) 0.8198(5) 0.9027(4) 0.0251(12) Uani 1 1 d . . .
H25 H 0.9706 0.8000 0.9211 0.030 Uiso 1 1 calc R . .
C26 C 0.93122(19) 0.9160(5) 0.8626(4) 0.0256(11) Uani 1 1 d . . .
H26 H 0.9514 0.9622 0.8531 0.031 Uiso 1 1 calc R . .
C27 C 0.88955(19) 0.9455(5) 0.8359(4) 0.0238(11) Uani 1 1 d . . .
H27 H 0.8817 1.0111 0.8068 0.029 Uiso 1 1 calc R . .
C28 C 0.86012(18) 0.8806(4) 0.8513(3) 0.0201(10) Uani 1 1 d . . .
H28 H 0.8323 0.9026 0.8338 0.024 Uiso 1 1 calc R . .
C1S C 0.58553(17) 0.5639(5) 0.9075(3) 0.0240(11) Uani 1 1 d . . .
H1S H 0.5888 0.5858 0.9724 0.029 Uiso 1 1 calc R . .
Cl2 Cl 0.54039(7) 0.48893(16) 0.86871(18) 0.0474(5) Uani 1 1 d . . .
Cl3 Cl 0.62859(6) 0.48924(12) 0.90582(13) 0.0301(3) Uani 1 1 d . . .
Cl4 Cl 0.58221(6) 0.67685(15) 0.83971(12) 0.0441(4) Uani 1 1 d . . .
C2S C 0.9201(5) 0.6960(15) 0.6787(13) 0.037(5) Uiso 0.39(2) 1 d PD A 1
H2S1 H 0.9108 0.7229 0.7296 0.056 Uiso 0.39(2) 1 calc PR A 1
H2S2 H 0.8993 0.6485 0.6409 0.056 Uiso 0.39(2) 1 calc PR A 1
H2S3 H 0.9243 0.7545 0.6408 0.056 Uiso 0.39(2) 1 calc PR A 1
C2S C 0.9287(5) 0.6834(14) 0.6352(11) 0.058(5) Uiso 0.61(2) 1 d PD A 2
H2S4 H 0.9158 0.6847 0.6851 0.087 Uiso 0.61(2) 1 calc PR A 2
H2S5 H 0.9124 0.6395 0.5848 0.087 Uiso 0.61(2) 1 calc PR A 2
H2S6 H 0.9300 0.7546 0.6126 0.087 Uiso 0.61(2) 1 calc PR A 2
C3S C 0.9615(5) 0.6355(14) 0.7186(14) 0.046(6) Uiso 0.39(2) 1 d PD A 1
H3S1 H 0.9595 0.5931 0.7716 0.055 Uiso 0.39(2) 1 calc PR A 1
H3S2 H 0.9648 0.5865 0.6709 0.055 Uiso 0.39(2) 1 calc PR A 1
C3S C 0.9706(6) 0.640(2) 0.6703(17) 0.117(9) Uiso 0.61(2) 1 d PD A 2
H3S3 H 0.9827 0.6368 0.6186 0.141 Uiso 0.61(2) 1 calc PR A 2
H3S4 H 0.9687 0.5680 0.6918 0.141 Uiso 0.61(2) 1 calc PR A 2
O1S O 1.0000 0.7033(15) 0.7500 0.133(7) Uani 1 2 d SD . .
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'
Cl Cl 0.1484 0.1585 '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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Re1 O2 103.17(17) . .
O1 Re1 O3 164.3(2) . .
O2 Re1 O3 84.99(16) . .
O1 Re1 N3 92.97(17) . .
O2 Re1 N3 163.84(15) . .
O3 Re1 N3 79.56(16) . .
O1 Re1 N1 86.6(2) . .
O2 Re1 N1 87.10(16) . .
O3 Re1 N1 80.37(16) . .
N3 Re1 N1 94.89(17) . .
O1 Re1 Cl1 101.53(17) . .
O2 Re1 Cl1 83.78(11) . .
O3 Re1 Cl1 92.63(11) . .
N3 Re1 Cl1 92.17(11) . .
N1 Re1 Cl1 168.97(13) . .
C1 O2 Re1 124.0(3) . .
C15 O3 Re1 125.5(3) . .
N2 N1 C7 106.6(4) . .
N2 N1 Re1 127.7(4) . .
C7 N1 Re1 122.9(3) . .
C9 N2 N1 110.7(4) . .
C9 N2 C10 126.0(4) . .
N1 N2 C10 123.1(4) . .
C21 N3 N4 105.8(4) . .
C21 N3 Re1 126.1(3) . .
N4 N3 Re1 127.8(3) . .
C23 N4 N3 110.6(4) . .
C23 N4 C24 126.8(5) . .
N3 N4 C24 122.4(4) . .
O2 C1 C6 126.2(5) . .
O2 C1 C2 114.6(5) . .
C6 C1 C2 119.2(5) . .
C3 C2 C1 120.5(5) . .
C2 C3 C4 121.8(5) . .
C11 C4 C5 121.0(5) . .
C11 C4 C3 121.0(5) . .
C5 C4 C3 118.0(5) . .
C4 C5 C6 120.3(5) . .
C4 C5 C14 116.6(5) . .
C6 C5 C14 122.9(5) . .
C1 C6 C5 119.7(5) . .
C1 C6 C7 119.4(5) . .
C5 C6 C7 120.7(4) . .
N1 C7 C8 108.6(5) . .
N1 C7 C6 123.2(4) . .
C8 C7 C6 128.3(5) . .
C9 C8 C7 106.1(5) . .
N2 C9 C8 108.0(5) . .
C12 C11 C4 120.7(6) . .
C11 C12 C13 119.5(6) . .
C14 C13 C12 120.7(6) . .
C13 C14 C5 121.3(6) . .
O3 C15 C20 121.4(5) . .
O3 C15 C16 117.9(5) . .
C20 C15 C16 120.7(5) . .
C17 C16 C15 120.6(5) . .
C16 C17 C18 120.3(5) . .
C25 C18 C19 119.9(5) . .
C25 C18 C17 120.5(5) . .
C19 C18 C17 119.6(5) . .
C28 C19 C18 117.8(5) . .
C28 C19 C20 123.5(5) . .
C18 C19 C20 118.6(5) . .
C15 C20 C19 119.6(5) . .
C15 C20 C21 118.9(5) . .
C19 C20 C21 121.5(4) . .
N3 C21 C22 109.5(5) . .
N3 C21 C20 121.5(4) . .
C22 C21 C20 128.8(5) . .
C23 C22 C21 105.8(5) . .
N4 C23 C22 108.3(5) . .
C26 C25 C18 120.8(6) . .
C25 C26 C27 119.6(5) . .
C28 C27 C26 120.9(5) . .
C27 C28 C19 121.0(5) . .
Cl3 C1S Cl4 110.4(3) . .
Cl3 C1S Cl2 110.6(4) . .
Cl4 C1S Cl2 110.7(3) . .
O1S C3S C2S 115.7(14) . .
C2S C3S O1S 115.0(15) . .
C3S O1S C3S 110.8(17) 2_756 .
C3S O1S C3S 33.2(11) 2_756 2_756
C3S O1S C3S 104.3(13) . 2_756
C3S O1S C3S 104.3(13) 2_756 .
C3S O1S C3S 33.2(11) . .
C3S O1S C3S 117(2) 2_756 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 O1 1.684(5) .
Re1 O2 1.977(4) .
Re1 O3 2.003(4) .
Re1 N3 2.117(4) .
Re1 N1 2.140(5) .
Re1 Cl1 2.3689(12) .
O2 C1 1.343(7) .
O3 C15 1.344(6) .
N1 N2 1.363(6) .
N1 C7 1.367(7) .
N2 C9 1.340(6) .
N2 C10 1.462(7) .
N3 C21 1.367(7) .
N3 N4 1.376(6) .
N4 C23 1.333(7) .
N4 C24 1.461(7) .
C1 C6 1.406(7) .
C1 C2 1.436(7) .
C2 C3 1.359(8) .
C3 C4 1.430(8) .
C4 C11 1.408(8) .
C4 C5 1.420(7) .
C5 C6 1.426(7) .
C5 C14 1.428(8) .
C6 C7 1.460(7) .
C7 C8 1.406(7) .
C8 C9 1.384(8) .
C11 C12 1.378(9) .
C12 C13 1.399(9) .
C13 C14 1.385(8) .
C15 C20 1.384(7) .
C15 C16 1.417(7) .
C16 C17 1.359(8) .
C17 C18 1.430(8) .
C18 C25 1.418(8) .
C18 C19 1.425(8) .
C19 C28 1.423(7) .
C19 C20 1.434(7) .
C20 C21 1.478(8) .
C21 C22 1.393(7) .
C22 C23 1.389(8) .
C25 C26 1.377(9) .
C26 C27 1.410(9) .
C27 C28 1.375(8) .
C1S Cl3 1.758(6) .
C1S Cl4 1.759(6) .
C1S Cl2 1.761(6) .
C2S C3S 1.567(16) .
C2S C3S 1.477(17) .
C3S O1S 1.528(16) .
C3S O1S 1.551(16) .
O1S C3S 1.528(16) 2_756
O1S C3S 1.551(16) 2_756
