
data_global


data_c:\users\steph\desktop\complex1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H23 Cl2 O Rh'
_chemical_formula_sum            'C14 H23 Cl2 O Rh'
_chemical_formula_weight         381.13

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'
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'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/n

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.7608(18)
_cell_length_b                   9.1868(15)
_cell_length_c                   13.945(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.291(10)
_cell_angle_gamma                90.00
_cell_volume                     1621.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8192
_cell_measurement_theta_min      2.314
_cell_measurement_theta_max      20.331

_exptl_crystal_description       fragment
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             776
_exptl_absorpt_coefficient_mu    1.370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3095
_exptl_absorpt_correction_T_max  0.8697
_exptl_absorpt_process_details   
;
Sheldrick, G.M. (2002). SADABS v. 2.03. University of Gottingen, Germany.
;
_exptl_special_details           
;
Rotating anode power 3.5 kW.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker X8 Apex diffractometer'
_diffrn_measurement_method       'Rotation images'
_diffrn_detector_area_resol_mean '120 microns'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            12362
_diffrn_reflns_av_R_equivalents  0.1384
_diffrn_reflns_av_sigmaI/netI    0.1172
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.31
_diffrn_reflns_theta_max         24.73
_reflns_number_total             2756
_reflns_number_gt                1515
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX 2 software, Bruker Nonius 2004'
_computing_cell_refinement       'APEX 2 software, Bruker Nonius 2004'
_computing_data_reduction        'SAINT, Bruker Nonius 2004'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'local program'

_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)+(0.1815P)²+9.5409P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2756
_refine_ls_number_parameters     168
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1717
_refine_ls_R_factor_gt           0.1103
_refine_ls_wR_factor_ref         0.3301
_refine_ls_wR_factor_gt          0.2833
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.211
_refine_ls_shift/su_mean         0.007

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
Rh1 Rh 0.10229(10) 0.04038(14) 0.42244(10) 0.0600(6) Uani 1 1 d . . .
Cl1 Cl 0.1214(4) -0.2205(5) 0.3948(5) 0.107(2) Uani 1 1 d . . .
O1 O 0.483(3) 0.798(9) 0.697(2) 0.55(3) Uani 1 1 d . . .
H1 H 0.4992 0.8671 0.6619 0.659 Uiso 1 1 calc R . .
C1 C 0.1875(15) 0.2418(17) 0.4537(14) 0.067(5) Uani 1 1 d . . .
Cl2 Cl 0.0923(3) -0.0098(5) 0.5949(4) 0.0729(14) Uani 1 1 d . . .
C2 C 0.2547(13) 0.1375(18) 0.4170(15) 0.064(5) Uani 1 1 d . . .
C3 C 0.2128(15) 0.0984(19) 0.3204(14) 0.070(5) Uani 1 1 d . . .
C4 C 0.1125(14) 0.1729(18) 0.2943(14) 0.071(6) Uani 1 1 d . . .
C5 C 0.1015(11) 0.2687(14) 0.3850(12) 0.045(4) Uani 1 1 d . . .
C6 C 0.3616(14) 0.081(2) 0.4741(16) 0.086(6) Uani 1 1 d . . .
H6A H 0.4094 0.1635 0.4901 0.129 Uiso 1 1 calc R . .
H6B H 0.3947 0.0114 0.4339 0.129 Uiso 1 1 calc R . .
H6C H 0.3472 0.0331 0.5338 0.129 Uiso 1 1 calc R . .
C7 C 0.264(2) -0.011(2) 0.2582(17) 0.102(8) Uani 1 1 d . . .
H7A H 0.2910 0.0401 0.2045 0.153 Uiso 1 1 calc R . .
H7B H 0.2122 -0.0839 0.2326 0.153 Uiso 1 1 calc R . .
H7C H 0.3233 -0.0594 0.2978 0.153 Uiso 1 1 calc R . .
C8 C 0.0429(15) 0.169(2) 0.2026(14) 0.079(6) Uani 1 1 d . . .
H8A H 0.0741 0.2266 0.1543 0.118 Uiso 1 1 calc R . .
H8B H -0.0261 0.2099 0.2118 0.118 Uiso 1 1 calc R . .
H8C H 0.0339 0.0681 0.1804 0.118 Uiso 1 1 calc R . .
C9 C 0.0073(14) 0.372(2) 0.3845(15) 0.074(5) Uani 1 1 d . . .
H9A H -0.0134 0.3773 0.4497 0.111 Uiso 1 1 calc R . .
H9B H -0.0521 0.3346 0.3396 0.111 Uiso 1 1 calc R . .
H9C H 0.0270 0.4686 0.3638 0.111 Uiso 1 1 calc R . .
C10 C 0.2070(14) 0.3246(19) 0.5475(15) 0.076(6) Uani 1 1 d . . .
H10A H 0.2445 0.2613 0.5981 0.091 Uiso 1 1 calc R . .
H10B H 0.1386 0.3531 0.5684 0.091 Uiso 1 1 calc R . .
C11 C 0.2772(19) 0.469(2) 0.5348(17) 0.092(7) Uani 1 1 d . . .
H11A H 0.3461 0.4386 0.5159 0.111 Uiso 1 1 calc R . .
H11B H 0.2408 0.5282 0.4812 0.111 Uiso 1 1 calc R . .
C12 C 0.2970(14) 0.562(2) 0.6214(15) 0.073(5) Uani 1 1 d . . .
H12A H 0.3351 0.5044 0.6748 0.087 Uiso 1 1 calc R . .
H12B H 0.2283 0.5916 0.6413 0.087 Uiso 1 1 calc R . .
C13 C 0.360(2) 0.697(3) 0.6072(16) 0.115(9) Uani 1 1 d . . .
H13A H 0.3184 0.7569 0.5571 0.138 Uiso 1 1 calc R . .
H13B H 0.4251 0.6663 0.5809 0.138 Uiso 1 1 calc R . .
C14 C 0.392(2) 0.793(3) 0.695(2) 0.125(9) Uani 1 1 d . . .
H14A H 0.3599 0.8909 0.6863 0.150 Uiso 1 1 calc R . .
H14B H 0.3720 0.7486 0.7547 0.150 Uiso 1 1 calc R . .


_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
Rh1 C2 2.150(14) . ?
Rh1 C5 2.161(13) . ?
Rh1 C1 2.163(16) . ?
Rh1 C4 2.180(17) . ?
Rh1 C3 2.193(14) . ?
Rh1 Cl1 2.444(5) . ?
Rh1 Cl2 2.468(5) . ?
Rh1 Cl2 2.480(4) 3_556 ?
O1 C14 1.16(4) . ?
O1 H1 0.8423 . ?
C1 C5 1.38(2) . ?
C1 C2 1.42(2) . ?
C1 C10 1.51(2) . ?
Cl2 Rh1 2.480(4) 3_556 ?
C2 C3 1.43(3) . ?
C2 C6 1.58(3) . ?
C3 C4 1.46(3) . ?
C3 C7 1.53(2) . ?
C4 C8 1.46(2) . ?
C4 C5 1.56(2) . ?
C5 C9 1.53(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.62(2) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.47(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.50(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.53(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?

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
C2 Rh1 C5 64.2(6) . . ?
C2 Rh1 C1 38.6(6) . . ?
C5 Rh1 C1 37.3(6) . . ?
C2 Rh1 C4 65.8(7) . . ?
C5 Rh1 C4 42.2(6) . . ?
C1 Rh1 C4 66.8(8) . . ?
C2 Rh1 C3 38.5(7) . . ?
C5 Rh1 C3 65.9(6) . . ?
C1 Rh1 C3 64.8(6) . . ?
C4 Rh1 C3 38.9(7) . . ?
C2 Rh1 Cl1 107.0(5) . . ?
C5 Rh1 Cl1 155.6(4) . . ?
C1 Rh1 Cl1 144.4(5) . . ?
C4 Rh1 Cl1 113.6(5) . . ?
C3 Rh1 Cl1 92.9(5) . . ?
C2 Rh1 Cl2 105.7(5) . . ?
C5 Rh1 Cl2 114.7(4) . . ?
C1 Rh1 Cl2 92.9(5) . . ?
C4 Rh1 Cl2 156.8(5) . . ?
C3 Rh1 Cl2 142.7(6) . . ?
Cl1 Rh1 Cl2 89.4(2) . . ?
C2 Rh1 Cl2 160.5(5) . 3_556 ?
C5 Rh1 Cl2 96.5(4) . 3_556 ?
C1 Rh1 Cl2 126.0(5) . 3_556 ?
C4 Rh1 Cl2 98.4(5) . 3_556 ?
C3 Rh1 Cl2 133.0(6) . 3_556 ?
Cl1 Rh1 Cl2 89.55(17) . 3_556 ?
Cl2 Rh1 Cl2 84.21(19) . 3_556 ?
C14 O1 H1 109.7 . . ?
C5 C1 C2 109.4(16) . . ?
C5 C1 C10 122.7(15) . . ?
C2 C1 C10 127.7(19) . . ?
C5 C1 Rh1 71.3(9) . . ?
C2 C1 Rh1 70.2(9) . . ?
C10 C1 Rh1 129.1(10) . . ?
Rh1 Cl2 Rh1 95.79(19) . 3_556 ?
C1 C2 C3 109.7(17) . . ?
C1 C2 C6 124.2(19) . . ?
C3 C2 C6 126.0(17) . . ?
C1 C2 Rh1 71.2(9) . . ?
C3 C2 Rh1 72.4(9) . . ?
C6 C2 Rh1 125.0(11) . . ?
C2 C3 C4 109.2(16) . . ?
C2 C3 C7 124.2(19) . . ?
C4 C3 C7 127(2) . . ?
C2 C3 Rh1 69.1(8) . . ?
C4 C3 Rh1 70.1(9) . . ?
C7 C3 Rh1 124.5(11) . . ?
C3 C4 C8 128.7(17) . . ?
C3 C4 C5 103.2(16) . . ?
C8 C4 C5 127.9(16) . . ?
C3 C4 Rh1 71.0(9) . . ?
C8 C4 Rh1 127.6(12) . . ?
C5 C4 Rh1 68.3(8) . . ?
C1 C5 C9 131.9(15) . . ?
C1 C5 C4 108.4(13) . . ?
C9 C5 C4 119.7(16) . . ?
C1 C5 Rh1 71.4(8) . . ?
C9 C5 Rh1 125.5(10) . . ?
C4 C5 Rh1 69.6(8) . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C3 C7 H7A 109.5 . . ?
C3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C9 H9A 109.5 . . ?
C5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C1 C10 C11 110.6(14) . . ?
C1 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C1 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
C12 C11 C10 115.1(16) . . ?
C12 C11 H11A 108.5 . . ?
C10 C11 H11A 108.5 . . ?
C12 C11 H11B 108.5 . . ?
C10 C11 H11B 108.5 . . ?
H11A C11 H11B 107.5 . . ?
C11 C12 C13 114.1(16) . . ?
C11 C12 H12A 108.7 . . ?
C13 C12 H12A 108.7 . . ?
C11 C12 H12B 108.7 . . ?
C13 C12 H12B 108.8 . . ?
H12A C12 H12B 107.6 . . ?
C12 C13 C14 117.8(19) . . ?
C12 C13 H13A 107.8 . . ?
C14 C13 H13A 107.8 . . ?
C12 C13 H13B 107.9 . . ?
C14 C13 H13B 107.9 . . ?
H13A C13 H13B 107.2 . . ?
O1 C14 C13 102(4) . . ?
O1 C14 H14A 111.6 . . ?
C13 C14 H14A 111.3 . . ?
O1 C14 H14B 111.2 . . ?
C13 C14 H14B 111.2 . . ?
H14A C14 H14B 109.2 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        24.73
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         2.260
_refine_diff_density_min         -1.859
_refine_diff_density_rms         0.210



