data_2010src0036
 
#Dr. Nick Fletcher/ Heather Montgomery

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C17 H15 Br Cl N2 O3 Re'
_chemical_formula_weight          596.87
 
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'
 'Br'  'Br'  -0.2901   2.4595
 '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'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    P2(1)/c
 
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'
 
_cell_length_a                    8.5959(2)
_cell_length_b                    13.7519(4)
_cell_length_c                    15.1599(5)
_cell_angle_alpha                 90.00
_cell_angle_beta                  92.572(2)
_cell_angle_gamma                 90.00
_cell_volume                      1790.25(9)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     4150
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        'Cut Blade'
_exptl_crystal_colour             Yellow
_exptl_crystal_size_max           0.26
_exptl_crystal_size_mid           0.13
_exptl_crystal_size_min           0.09
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.215
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1128
_exptl_absorpt_coefficient_mu     9.187
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.1986
_exptl_absorpt_correction_T_max   0.4919
_exptl_absorpt_process_details       'SADABS 2007/2 (Sheldrick, G.M., 2007)'

_exptl_special_details
;
SADABS was used to perform the Absorption correction
Estimated minimum and maximum transmission: 0.4882 0.7456
The given Tmin and Tmax were generated using the SHELX SIZE command
;


_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    'graphite'
_diffrn_measurement_device_type   
'Bruker-Nonius Roper CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   '9.091'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             20565
_diffrn_reflns_av_R_equivalents   0.0449
_diffrn_reflns_av_sigmaI/netI     0.0378
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -18
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          3.25
_diffrn_reflns_theta_max          27.48
_reflns_number_total              4090
_reflns_number_gt                 3471
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material   'WinGX (Farrugia, 1999)'
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0251P)²+8.9538P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.00109(15)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          4090
_refine_ls_number_parameters      255
_refine_ls_number_restraints      45
_refine_ls_R_factor_all           0.0441
_refine_ls_R_factor_gt            0.0334
_refine_ls_wR_factor_ref          0.0774
_refine_ls_wR_factor_gt           0.0734
_refine_ls_goodness_of_fit_ref    1.074
_refine_ls_restrained_S_all       1.071
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
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 0.83900(2) 0.536010(14) 0.188629(15) 0.02480(10) Uani 1 1 d D . .
C1 C 0.5911(7) 0.7034(4) 0.1901(4) 0.0319(13) Uani 1 1 d . . .
H1 H 0.6757 0.7410 0.2137 0.038 Uiso 1 1 calc R A .
C2 C 0.4462(8) 0.7473(4) 0.1783(4) 0.0394(15) Uani 1 1 d . A .
H2 H 0.4314 0.8133 0.1943 0.047 Uiso 1 1 calc R . .
C3 C 0.3238(7) 0.6925(5) 0.1427(4) 0.0396(15) Uani 1 1 d . . .
H3 H 0.2240 0.7211 0.1325 0.047 Uiso 1 1 calc R A .
C4 C 0.3478(6) 0.5965(5) 0.1221(4) 0.0337(13) Uani 1 1 d . A .
H4 H 0.2641 0.5581 0.0983 0.040 Uiso 1 1 calc R . .
C5 C 0.4946(6) 0.5558(4) 0.1360(4) 0.0285(12) Uani 1 1 d . . .
C6 C 0.5318(6) 0.4537(4) 0.1145(4) 0.0254(11) Uani 1 1 d . A .
C7 C 0.4225(6) 0.3865(5) 0.0835(4) 0.0336(13) Uani 1 1 d . . .
H7 H 0.3163 0.4050 0.0754 0.040 Uiso 1 1 calc R A .
C8 C 0.4672(7) 0.2933(5) 0.0643(4) 0.0351(14) Uani 1 1 d . A .
H8 H 0.3916 0.2469 0.0444 0.042 Uiso 1 1 calc R . .
C9 C 0.6233(7) 0.2668(4) 0.0741(4) 0.0312(12) Uani 1 1 d . . .
C10 C 0.7271(6) 0.3372(4) 0.1057(4) 0.0265(12) Uani 1 1 d . A .
H10 H 0.8340 0.3204 0.1134 0.032 Uiso 1 1 calc R . .
C11 C 0.6781(7) 0.1665(4) 0.0516(4) 0.0353(14) Uani 1 1 d . A .
H11A H 0.7915 0.1684 0.0430 0.042 Uiso 1 1 calc R . .
H11B H 0.6258 0.1457 -0.0048 0.042 Uiso 1 1 calc R . .
C12 C 0.6452(7) 0.0921(4) 0.1228(4) 0.0392(14) Uani 1 1 d . . .
H12A H 0.5340 0.0967 0.1367 0.047 Uiso 1 1 calc R A .
H12B H 0.7079 0.1089 0.1770 0.047 Uiso 1 1 calc R . .
C13 C 0.6810(8) -0.0133(4) 0.0977(5) 0.0412(15) Uani 1 1 d . A .
H13A H 0.6630 -0.0561 0.1488 0.049 Uiso 1 1 calc R . .
H13B H 0.6085 -0.0336 0.0485 0.049 Uiso 1 1 calc R . .
C14 C 0.8425(7) -0.0260(4) 0.0708(5) 0.0383(15) Uani 1 1 d . . .
H14A H 0.9152 -0.0001 0.1176 0.046 Uiso 1 1 calc R A .
H14B H 0.8578 0.0114 0.0161 0.046 Uiso 1 1 calc R . .
N1 N 0.6168(5) 0.6096(3) 0.1695(3) 0.0259(10) Uani 1 1 d . A .
N2 N 0.6836(5) 0.4284(3) 0.1261(3) 0.0229(9) Uani 1 1 d . A .
Br1 Br 0.88974(8) -0.16355(5) 0.05028(5) 0.04458(18) Uani 1 1 d . A .
C21 C 1.0220(6) 0.4562(4) 0.2024(4) 0.0296(12) Uani 1 1 d D A .
O21 O 1.1316(4) 0.4077(3) 0.2095(3) 0.0364(10) Uani 1 1 d . . .
C31 C 0.9505(7) 0.6397(4) 0.2485(4) 0.0325(13) Uani 1 1 d D A .
O31 O 1.0153(5) 0.7014(3) 0.2858(3) 0.0474(12) Uani 1 1 d . . .
C41 C 0.907(2) 0.5844(13) 0.0770(8) 0.025(3) Uani 0.735(13) 1 d PDU A 1
O41 O 0.9580(10) 0.6132(6) 0.0141(6) 0.0331(16) Uani 0.735(13) 1 d PU A 1
Cl41 Cl 0.9185(12) 0.5895(8) 0.0456(5) 0.020(2) Uani 0.265(13) 1 d PDU A 2
C51 C 0.770(3) 0.487(2) 0.3009(14) 0.017(4) Uani 0.265(13) 1 d PDU A 2
O51 O 0.734(2) 0.4685(15) 0.3646(16) 0.016(3) Uani 0.265(13) 1 d PU A 2
Cl51 Cl 0.7360(3) 0.47879(18) 0.32759(19) 0.0240(10) Uani 0.735(13) 1 d PDU A 1
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
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
Re1 C21 1.922(6) . ?
Re1 C31 1.923(6) . ?
Re1 C41 1.934(11) . ?
Re1 C51 1.949(15) . ?
Re1 N1 2.169(4) . ?
Re1 N2 2.181(4) . ?
Re1 Cl41 2.417(8) . ?
Re1 Cl51 2.451(3) . ?
C1 N1 1.348(7) . ?
C1 C2 1.389(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.384(10) . ?
C2 H2 0.9500 . ?
C3 C4 1.375(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.388(8) . ?
C4 H4 0.9500 . ?
C5 N1 1.364(7) . ?
C5 C6 1.479(8) . ?
C6 N2 1.354(7) . ?
C6 C7 1.385(8) . ?
C7 C8 1.374(9) . ?
C7 H7 0.9500 . ?
C8 C9 1.392(8) . ?
C8 H8 0.9500 . ?
C9 C10 1.388(7) . ?
C9 C11 1.501(8) . ?
C10 N2 1.349(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.522(8) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.533(9) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.475(9) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 Br1 1.962(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C21 O21 1.155(6) . ?
C31 O31 1.150(7) . ?
C41 O41 1.137(17) . ?
C51 O51 1.06(3) . ?
 
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
C21 Re1 C31 89.1(2) . . ?
C21 Re1 C41 90.7(6) . . ?
C31 Re1 C41 89.7(6) . . ?
C21 Re1 C51 89.2(9) . . ?
C31 Re1 C51 90.6(10) . . ?
C41 Re1 C51 179.7(11) . . ?
C21 Re1 N1 172.90(19) . . ?
C31 Re1 N1 97.7(2) . . ?
C41 Re1 N1 91.2(6) . . ?
C51 Re1 N1 88.8(9) . . ?
C21 Re1 N2 98.2(2) . . ?
C31 Re1 N2 172.1(2) . . ?
C41 Re1 N2 93.2(5) . . ?
C51 Re1 N2 86.5(10) . . ?
N1 Re1 N2 74.91(16) . . ?
C21 Re1 Cl41 90.5(3) . . ?
C31 Re1 Cl41 92.5(3) . . ?
C41 Re1 Cl41 2.8(7) . . ?
C51 Re1 Cl41 176.9(10) . . ?
N1 Re1 Cl41 91.2(3) . . ?
N2 Re1 Cl41 90.5(3) . . ?
C21 Re1 Cl51 92.80(19) . . ?
C31 Re1 Cl51 91.37(19) . . ?
C41 Re1 Cl51 176.3(6) . . ?
C51 Re1 Cl51 3.7(9) . . ?
N1 Re1 Cl51 85.12(13) . . ?
N2 Re1 Cl51 85.28(13) . . ?
Cl41 Re1 Cl51 175.0(3) . . ?
N1 C1 C2 122.8(6) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C3 C2 C1 118.4(6) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C4 C3 C2 119.5(6) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 119.8(6) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
N1 C5 C4 121.2(5) . . ?
N1 C5 C6 115.2(5) . . ?
C4 C5 C6 123.6(6) . . ?
N2 C6 C7 120.5(5) . . ?
N2 C6 C5 115.6(5) . . ?
C7 C6 C5 123.9(5) . . ?
C8 C7 C6 120.2(5) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C7 C8 C9 119.9(5) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C10 C9 C8 117.1(5) . . ?
C10 C9 C11 121.1(5) . . ?
C8 C9 C11 121.8(5) . . ?
N2 C10 C9 123.2(5) . . ?
N2 C10 H10 118.4 . . ?
C9 C10 H10 118.4 . . ?
C9 C11 C12 112.7(5) . . ?
C9 C11 H11A 109.0 . . ?
C12 C11 H11A 109.0 . . ?
C9 C11 H11B 109.0 . . ?
C12 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 C13 114.5(5) . . ?
C11 C12 H12A 108.6 . . ?
C13 C12 H12A 108.6 . . ?
C11 C12 H12B 108.6 . . ?
C13 C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
C14 C13 C12 112.5(5) . . ?
C14 C13 H13A 109.1 . . ?
C12 C13 H13A 109.1 . . ?
C14 C13 H13B 109.1 . . ?
C12 C13 H13B 109.1 . . ?
H13A C13 H13B 107.8 . . ?
C13 C14 Br1 111.2(4) . . ?
C13 C14 H14A 109.4 . . ?
Br1 C14 H14A 109.4 . . ?
C13 C14 H14B 109.4 . . ?
Br1 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C1 N1 C5 118.3(5) . . ?
C1 N1 Re1 124.6(4) . . ?
C5 N1 Re1 117.1(3) . . ?
C10 N2 C6 119.0(5) . . ?
C10 N2 Re1 124.0(3) . . ?
C6 N2 Re1 116.8(3) . . ?
O21 C21 Re1 179.1(5) . . ?
O31 C31 Re1 178.6(6) . . ?
O41 C41 Re1 174.9(16) . . ?
O51 C51 Re1 173(3) . . ?
 
_diffrn_measured_fraction_theta_max    0.998
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.998
_refine_diff_density_max    1.220
_refine_diff_density_min   -1.402
_refine_diff_density_rms    0.159
