 
data_2007src0942 

#Dr Annabelle Hodson
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C23 H18 Cl Mo N3 O3' 
_chemical_formula_weight          515.79 
 
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' 
 'Mo'  'Mo'  -1.6832   0.6857 
 '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                    9.2976(2) 
_cell_length_b                    27.3184(5) 
_cell_length_c                    8.7746(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  107.8340(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      2121.61(8) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     120(2) 
_cell_measurement_reflns_used    42877
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description       Block 
_exptl_crystal_colour             Orange
_exptl_crystal_size_max           0.18 
_exptl_crystal_size_mid           0.04 
_exptl_crystal_size_min           0.01 
_exptl_crystal_density_meas        'not measured' 
_exptl_crystal_density_diffrn     1.615 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1040 
_exptl_absorpt_coefficient_mu     0.775 
_exptl_absorpt_correction_type    Multi-scan 
_exptl_absorpt_correction_T_min   0.8731 
_exptl_absorpt_correction_T_max   0.9923 
_exptl_absorpt_process_details    'SADABS V2.10 (Sheldrick, G.M., 2003)' 
 
_exptl_special_details 
; 
SADABS was used to perform the Absorption correction 
Parameter refinement on 24375 reflections reduced R(int) from 0.1062 to 0.0412 
Ratio of minimum to maximum apparent transmission: 0.894015 
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   '10cm confocal mirrors' 
_diffrn_measurement_device_type  'Bruker-Nonius 95mm 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             24408 
_diffrn_reflns_av_R_equivalents   0.0375 
_diffrn_reflns_av_sigmaI/netI     0.0313 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -35 
_diffrn_reflns_limit_k_max        35 
_diffrn_reflns_limit_l_min        -11 
_diffrn_reflns_limit_l_max        11 
_diffrn_reflns_theta_min          3.17 
_diffrn_reflns_theta_max          27.48 
_reflns_number_total              4835 
_reflns_number_gt                 4434 
_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, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
 
_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)+(0.0000P)²+8.0214P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          4835 
_refine_ls_number_parameters      288 
_refine_ls_number_restraints      6 
_refine_ls_R_factor_all           0.0520 
_refine_ls_R_factor_gt            0.0461 
_refine_ls_wR_factor_ref          0.0982 
_refine_ls_wR_factor_gt           0.0953 
_refine_ls_goodness_of_fit_ref    1.201 
_refine_ls_restrained_S_all       1.203 
_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 
Mo Mo 0.58763(3) 0.133079(11) 0.37185(4) 0.01725(9) Uani 1 1 d . . . 
Cl1 Cl 0.62086(10) 0.16617(3) 0.64340(10) 0.02174(18) Uani 1 1 d . . . 
C1 C 0.7934(4) 0.04416(13) 0.5575(4) 0.0205(7) Uani 1 1 d . . . 
H1 H 0.7008 0.0266 0.5329 0.025 Uiso 1 1 calc R . . 
C2 C 0.9247(4) 0.02091(13) 0.6500(4) 0.0234(7) Uani 1 1 d . . . 
H2 H 0.9206 -0.0115 0.6875 0.028 Uiso 1 1 calc R . . 
C3 C 1.0604(4) 0.04539(13) 0.6863(4) 0.0231(8) Uani 1 1 d . . . 
H3 H 1.1511 0.0300 0.7484 0.028 Uiso 1 1 calc R . . 
C4 C 1.0626(4) 0.09340(13) 0.6301(4) 0.0203(7) Uani 1 1 d . . . 
C5 C 0.9256(4) 0.11384(12) 0.5368(4) 0.0165(6) Uani 1 1 d . . . 
C6 C 1.1977(4) 0.12224(13) 0.6636(5) 0.0235(8) Uani 1 1 d . . . 
H6 H 1.2901 0.1091 0.7303 0.028 Uiso 1 1 calc R . . 
C7 C 1.1964(4) 0.16779(15) 0.6022(5) 0.0260(8) Uani 1 1 d . . . 
H7 H 1.2877 0.1860 0.6254 0.031 Uiso 1 1 calc R . . 
C8 C 1.0587(4) 0.18867(13) 0.5028(4) 0.0211(7) Uani 1 1 d . . . 
C9 C 0.9231(4) 0.16239(12) 0.4735(4) 0.0175(7) Uani 1 1 d . . . 
C10 C 1.0505(4) 0.23561(13) 0.4324(5) 0.0243(8) Uani 1 1 d . . . 
H10 H 1.1393 0.2547 0.4480 0.029 Uiso 1 1 calc R . . 
C11 C 0.9139(4) 0.25324(14) 0.3418(5) 0.0261(8) Uani 1 1 d . . . 
H11 H 0.9071 0.2846 0.2931 0.031 Uiso 1 1 calc R . . 
C12 C 0.7836(4) 0.22493(13) 0.3209(5) 0.0250(8) Uani 1 1 d . . . 
H12 H 0.6891 0.2380 0.2592 0.030 Uiso 1 1 calc R . . 
C13 C 0.4252(4) 0.18272(14) 0.3028(5) 0.0253(8) Uani 1 1 d . . . 
C14 C 0.4251(4) 0.09208(14) 0.4105(4) 0.0216(7) Uani 1 1 d . . . 
C15 C 0.4887(4) 0.18241(15) 0.0024(5) 0.0288(8) Uani 1 1 d . . . 
H15A H 0.5089 0.1792 -0.0968 0.035 Uiso 1 1 calc R . . 
H15B H 0.4360 0.2103 0.0221 0.035 Uiso 1 1 calc R . . 
C16 C 0.5338(4) 0.14823(13) 0.1128(4) 0.0211(7) Uani 1 1 d . . . 
C17 C 0.6106(4) 0.10287(13) 0.1423(4) 0.0205(7) Uani 1 1 d . . . 
C18 C 0.5346(4) 0.06832(14) 0.2094(4) 0.0233(7) Uani 1 1 d . . . 
C19 C 0.4845(5) 0.02420(15) 0.1981(5) 0.0303(9) Uani 1 1 d D . . 
C20 C 0.4230(7) -0.01847(19) 0.1883(6) 0.0451(12) Uani 1 1 d D . . 
C21 C 0.7623(4) 0.09172(13) 0.1227(4) 0.0221(7) Uani 1 1 d . . . 
C22 C 0.9399(5) 0.11160(16) -0.0219(5) 0.0313(9) Uani 1 1 d . . . 
H22A H 0.9296 0.1267 -0.1273 0.038 Uiso 1 1 calc R . . 
H22B H 0.9506 0.0758 -0.0325 0.038 Uiso 1 1 calc R . . 
C23 C 1.0787(5) 0.1310(2) 0.0982(6) 0.0461(12) Uani 1 1 d . . . 
H23A H 1.1671 0.1234 0.0640 0.069 Uiso 1 1 calc R . . 
H23B H 1.0903 0.1158 0.2025 0.069 Uiso 1 1 calc R . . 
H23C H 1.0700 0.1666 0.1070 0.069 Uiso 1 1 calc R . . 
O1 O 0.3355(3) 0.21288(11) 0.2640(4) 0.0354(7) Uani 1 1 d . . . 
O2 O 0.3339(3) 0.06804(10) 0.4334(3) 0.0303(6) Uani 1 1 d . . . 
O3 O 0.8379(3) 0.05663(10) 0.1878(3) 0.0295(6) Uani 1 1 d . . . 
N1 N 0.7909(3) 0.08954(10) 0.5018(3) 0.0172(6) Uani 1 1 d . . . 
N2 N 0.7868(3) 0.18036(10) 0.3840(4) 0.0180(6) Uani 1 1 d . . . 
N3 N 0.8034(4) 0.12151(12) 0.0224(4) 0.0281(7) Uani 1 1 d . . . 
H3A H 0.7478 0.1473 -0.0173 0.034 Uiso 1 1 calc R . . 
H20A H 0.320(2) -0.0179(17) 0.136(6) 0.09(2) Uiso 1 1 d D . . 
H20B H 0.497(4) -0.0416(12) 0.234(6) 0.08(2) Uiso 1 1 d D . . 
 
 
_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 
Mo C13 1.982(4) . ? 
Mo C14 1.991(4) . ? 
Mo C16 2.211(4) . ? 
Mo N1 2.229(3) . ? 
Mo C18 2.230(4) . ? 
Mo N2 2.233(3) . ? 
Mo C17 2.247(3) . ? 
Mo Cl1 2.4778(9) . ? 
C1 N1 1.330(4) . ? 
C1 C2 1.395(5) . ? 
C1 H1 0.9500 . ? 
C2 C3 1.376(5) . ? 
C2 H2 0.9500 . ? 
C3 C4 1.403(5) . ? 
C3 H3 0.9500 . ? 
C4 C5 1.403(5) . ? 
C4 C6 1.435(5) . ? 
C5 N1 1.366(4) . ? 
C5 C9 1.436(5) . ? 
C6 C7 1.354(5) . ? 
C6 H6 0.9500 . ? 
C7 C8 1.428(5) . ? 
C7 H7 0.9500 . ? 
C8 C9 1.404(5) . ? 
C8 C10 1.416(5) . ? 
C9 N2 1.362(4) . ? 
C10 C11 1.363(5) . ? 
C10 H10 0.9500 . ? 
C11 C12 1.401(5) . ? 
C11 H11 0.9500 . ? 
C12 N2 1.334(4) . ? 
C12 H12 0.9500 . ? 
C13 O1 1.147(5) . ? 
C14 O2 1.139(4) . ? 
C15 C16 1.318(5) . ? 
C15 H15A 0.9500 . ? 
C15 H15B 0.9500 . ? 
C16 C17 1.414(5) . ? 
C17 C18 1.412(5) . ? 
C17 C21 1.504(5) . ? 
C18 C19 1.285(5) . ? 
C19 C20 1.290(6) . ? 
C20 H20A 0.922(18) . ? 
C20 H20B 0.930(18) . ? 
C21 O3 1.222(4) . ? 
C21 N3 1.338(5) . ? 
C22 N3 1.462(5) . ? 
C22 C23 1.491(6) . ? 
C22 H22A 0.9900 . ? 
C22 H22B 0.9900 . ? 
C23 H23A 0.9800 . ? 
C23 H23B 0.9800 . ? 
C23 H23C 0.9800 . ? 
N3 H3A 0.8800 . ? 
 
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 
C13 Mo C14 83.68(15) . . ? 
C13 Mo C16 69.28(15) . . ? 
C14 Mo C16 109.59(14) . . ? 
C13 Mo N1 165.73(13) . . ? 
C14 Mo N1 100.46(13) . . ? 
C16 Mo N1 121.02(12) . . ? 
C13 Mo C18 110.42(15) . . ? 
C14 Mo C18 68.39(14) . . ? 
C16 Mo C18 63.62(14) . . ? 
N1 Mo C18 83.72(12) . . ? 
C13 Mo N2 99.32(13) . . ? 
C14 Mo N2 168.05(13) . . ? 
C16 Mo N2 82.21(12) . . ? 
N1 Mo N2 73.94(10) . . ? 
C18 Mo N2 120.49(12) . . ? 
C13 Mo C17 104.49(15) . . ? 
C14 Mo C17 103.38(14) . . ? 
C16 Mo C17 36.97(13) . . ? 
N1 Mo C17 87.95(12) . . ? 
C18 Mo C17 36.76(13) . . ? 
N2 Mo C17 87.15(12) . . ? 
C13 Mo Cl1 84.44(11) . . ? 
C14 Mo Cl1 85.37(10) . . ? 
C16 Mo Cl1 147.39(10) . . ? 
N1 Mo Cl1 82.31(8) . . ? 
C18 Mo Cl1 147.35(10) . . ? 
N2 Mo Cl1 83.43(8) . . ? 
C17 Mo Cl1 167.99(9) . . ? 
N1 C1 C2 123.5(3) . . ? 
N1 C1 H1 118.3 . . ? 
C2 C1 H1 118.3 . . ? 
C3 C2 C1 119.4(3) . . ? 
C3 C2 H2 120.3 . . ? 
C1 C2 H2 120.3 . . ? 
C2 C3 C4 118.9(3) . . ? 
C2 C3 H3 120.5 . . ? 
C4 C3 H3 120.5 . . ? 
C5 C4 C3 118.0(3) . . ? 
C5 C4 C6 118.9(3) . . ? 
C3 C4 C6 123.2(3) . . ? 
N1 C5 C4 122.9(3) . . ? 
N1 C5 C9 117.2(3) . . ? 
C4 C5 C9 119.8(3) . . ? 
C7 C6 C4 121.5(3) . . ? 
C7 C6 H6 119.2 . . ? 
C4 C6 H6 119.2 . . ? 
C6 C7 C8 120.4(3) . . ? 
C6 C7 H7 119.8 . . ? 
C8 C7 H7 119.8 . . ? 
C9 C8 C10 117.2(3) . . ? 
C9 C8 C7 119.6(3) . . ? 
C10 C8 C7 123.2(3) . . ? 
N2 C9 C8 123.1(3) . . ? 
N2 C9 C5 117.2(3) . . ? 
C8 C9 C5 119.6(3) . . ? 
C11 C10 C8 119.4(3) . . ? 
C11 C10 H10 120.3 . . ? 
C8 C10 H10 120.3 . . ? 
C10 C11 C12 119.7(3) . . ? 
C10 C11 H11 120.2 . . ? 
C12 C11 H11 120.2 . . ? 
N2 C12 C11 122.7(3) . . ? 
N2 C12 H12 118.6 . . ? 
C11 C12 H12 118.6 . . ? 
O1 C13 Mo 177.3(3) . . ? 
O2 C14 Mo 178.9(3) . . ? 
C16 C15 H15A 120.0 . . ? 
C16 C15 H15B 120.0 . . ? 
H15A C15 H15B 120.0 . . ? 
C15 C16 C17 141.6(4) . . ? 
C15 C16 Mo 144.0(3) . . ? 
C17 C16 Mo 72.9(2) . . ? 
C18 C17 C16 111.9(3) . . ? 
C18 C17 C21 121.3(3) . . ? 
C16 C17 C21 126.6(3) . . ? 
C18 C17 Mo 71.0(2) . . ? 
C16 C17 Mo 70.1(2) . . ? 
C21 C17 Mo 121.8(2) . . ? 
C19 C18 C17 144.2(4) . . ? 
C19 C18 Mo 142.9(3) . . ? 
C17 C18 Mo 72.3(2) . . ? 
C18 C19 C20 174.8(5) . . ? 
C19 C20 H20A 113(3) . . ? 
C19 C20 H20B 109(3) . . ? 
H20A C20 H20B 138(4) . . ? 
O3 C21 N3 123.1(3) . . ? 
O3 C21 C17 122.1(3) . . ? 
N3 C21 C17 114.8(3) . . ? 
N3 C22 C23 112.3(4) . . ? 
N3 C22 H22A 109.1 . . ? 
C23 C22 H22A 109.1 . . ? 
N3 C22 H22B 109.1 . . ? 
C23 C22 H22B 109.1 . . ? 
H22A C22 H22B 107.9 . . ? 
C22 C23 H23A 109.5 . . ? 
C22 C23 H23B 109.5 . . ? 
H23A C23 H23B 109.5 . . ? 
C22 C23 H23C 109.5 . . ? 
H23A C23 H23C 109.5 . . ? 
H23B C23 H23C 109.5 . . ? 
C1 N1 C5 117.3(3) . . ? 
C1 N1 Mo 127.0(2) . . ? 
C5 N1 Mo 115.5(2) . . ? 
C12 N2 C9 117.8(3) . . ? 
C12 N2 Mo 126.5(2) . . ? 
C9 N2 Mo 115.5(2) . . ? 
C21 N3 C22 120.6(3) . . ? 
C21 N3 H3A 119.7 . . ? 
C22 N3 H3A 119.7 . . ? 
 
_diffrn_measured_fraction_theta_max    0.996 
_diffrn_reflns_theta_full              27.48 
_diffrn_measured_fraction_theta_full   0.996 
_refine_diff_density_max    1.010 
_refine_diff_density_min   -0.629 
_refine_diff_density_rms    0.098 
