data_2008src0770
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C27 H34 Cl N2 Rh'
_chemical_formula_weight          524.92
 
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'
 '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    P2(1)/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                    11.46310(10)
_cell_length_b                    12.2418(2)
_cell_length_c                    17.1604(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  95.5550(10)
_cell_angle_gamma                 90.00
_cell_volume                      2396.79(5)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     46339
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        plate
_exptl_crystal_colour             yellow
_exptl_crystal_size_max           0.40
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.03
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.455
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1088
_exptl_absorpt_coefficient_mu     0.841
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.7297
_exptl_absorpt_correction_T_max   0.9752
_exptl_absorpt_process_details    'SADABS V2.10 (Sheldrick, G.M., 2003)'
 
_exptl_special_details
;
 ?
;
 
_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 APEX2 Area Detector'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          none
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         negligible
_diffrn_reflns_number             29481
_diffrn_reflns_av_R_equivalents   0.0360
_diffrn_reflns_av_sigmaI/netI     0.0269
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -22
_diffrn_reflns_limit_l_max        22
_diffrn_reflns_theta_min          2.91
_diffrn_reflns_theta_max          27.48
_reflns_number_total              5483
_reflns_number_gt                 5100
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        ?
_computing_cell_refinement        'DENZO, COLLECT'
_computing_data_reduction         'DENZO, COLLECT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'PLATON (Spek, 2003)'
_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)+(0.0496P)²+9.0090P] 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          5483
_refine_ls_number_parameters      280
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0421
_refine_ls_R_factor_gt            0.0387
_refine_ls_wR_factor_ref          0.1103
_refine_ls_wR_factor_gt           0.1069
_refine_ls_goodness_of_fit_ref    1.056
_refine_ls_restrained_S_all       1.056
_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
C1 C 1.0928(3) 0.2499(2) 0.22003(17) 0.0136(5) Uani 1 1 d . . .
C2 C 1.0528(3) 0.2424(3) 0.35448(18) 0.0181(6) Uani 1 1 d . . .
C3 C 1.0160(3) 0.3397(3) 0.3853(2) 0.0248(7) Uani 1 1 d . . .
H3 H 1.0447 0.4074 0.3681 0.030 Uiso 1 1 calc R . .
C4 C 0.9369(3) 0.3376(4) 0.4416(2) 0.0312(8) Uani 1 1 d . . .
H4 H 0.9110 0.4042 0.4627 0.037 Uiso 1 1 calc R . .
C5 C 0.8957(3) 0.2396(4) 0.4671(2) 0.0313(8) Uani 1 1 d . . .
H5 H 0.8403 0.2384 0.5049 0.038 Uiso 1 1 calc R . .
C6 C 0.9354(3) 0.1426(3) 0.4375(2) 0.0282(8) Uani 1 1 d . . .
H6 H 0.9074 0.0752 0.4558 0.034 Uiso 1 1 calc R . .
C7 C 1.0157(3) 0.1422(3) 0.38116(19) 0.0215(6) Uani 1 1 d . . .
C8 C 1.0593(4) 0.0357(3) 0.3515(2) 0.0305(8) Uani 1 1 d . . .
H8A H 1.1146 0.0501 0.3126 0.046 Uiso 1 1 calc R . .
H8B H 0.9930 -0.0068 0.3273 0.046 Uiso 1 1 calc R . .
H8C H 1.0989 -0.0057 0.3952 0.046 Uiso 1 1 calc R . .
C9 C 1.2598(3) 0.2630(3) 0.33015(19) 0.0223(7) Uani 1 1 d . . .
H9A H 1.2983 0.1915 0.3414 0.027 Uiso 1 1 calc R . .
H9B H 1.2588 0.3026 0.3803 0.027 Uiso 1 1 calc R . .
C10 C 1.3313(3) 0.3282(3) 0.2759(2) 0.0205(6) Uani 1 1 d . . .
H10A H 1.4000 0.3607 0.3069 0.025 Uiso 1 1 calc R . .
H10B H 1.2827 0.3887 0.2521 0.025 Uiso 1 1 calc R . .
C11 C 1.3735(3) 0.2574(3) 0.2109(2) 0.0213(6) Uani 1 1 d . . .
H11A H 1.3887 0.3040 0.1658 0.026 Uiso 1 1 calc R . .
H11B H 1.4478 0.2208 0.2302 0.026 Uiso 1 1 calc R . .
C12 C 1.2821(3) 0.1722(3) 0.18489(19) 0.0188(6) Uani 1 1 d . . .
H12A H 1.3060 0.1337 0.1383 0.023 Uiso 1 1 calc R . .
H12B H 1.2781 0.1176 0.2271 0.023 Uiso 1 1 calc R . .
C13 C 1.1308(3) 0.2393(3) 0.08362(17) 0.0162(6) Uani 1 1 d . . .
C14 C 1.1220(3) 0.1509(3) 0.03147(18) 0.0172(6) Uani 1 1 d . . .
C15 C 1.1430(3) 0.0339(3) 0.0572(2) 0.0236(7) Uani 1 1 d . . .
H15A H 1.1643 0.0317 0.1138 0.035 Uiso 1 1 calc R . .
H15B H 1.2068 0.0030 0.0301 0.035 Uiso 1 1 calc R . .
H15C H 1.0714 -0.0088 0.0442 0.035 Uiso 1 1 calc R . .
C16 C 1.0906(3) 0.1732(3) -0.04750(19) 0.0212(7) Uani 1 1 d . . .
H16 H 1.0851 0.1145 -0.0839 0.025 Uiso 1 1 calc R . .
C17 C 1.0674(3) 0.2782(3) -0.07433(19) 0.0227(7) Uani 1 1 d . . .
H17 H 1.0454 0.2910 -0.1284 0.027 Uiso 1 1 calc R . .
C18 C 1.0762(3) 0.3646(3) -0.02210(19) 0.0230(7) Uani 1 1 d . . .
H18 H 1.0596 0.4368 -0.0401 0.028 Uiso 1 1 calc R . .
C19 C 1.1097(3) 0.3454(3) 0.05695(19) 0.0194(6) Uani 1 1 d . . .
H19 H 1.1181 0.4049 0.0926 0.023 Uiso 1 1 calc R . .
C20 C 0.8326(3) 0.1756(2) 0.20861(19) 0.0179(6) Uani 1 1 d . . .
H20 H 0.8921 0.1549 0.2483 0.022 Uiso 1 1 calc R . .
C21 C 0.8627(3) 0.1818(3) 0.1311(2) 0.0196(6) Uani 1 1 d . . .
H21 H 0.9401 0.1610 0.1221 0.024 Uiso 1 1 calc R . .
C22 C 0.7825(3) 0.2187(4) 0.0608(2) 0.0308(8) Uani 1 1 d . . .
H22A H 0.7291 0.1579 0.0436 0.037 Uiso 1 1 calc R . .
H22B H 0.8305 0.2354 0.0173 0.037 Uiso 1 1 calc R . .
C23 C 0.7094(3) 0.3189(4) 0.0767(2) 0.0328(9) Uani 1 1 d . . .
H23A H 0.6874 0.3575 0.0267 0.039 Uiso 1 1 calc R . .
H23B H 0.6363 0.2950 0.0979 0.039 Uiso 1 1 calc R . .
C24 C 0.7741(3) 0.3974(3) 0.1339(2) 0.0240(7) Uani 1 1 d . . .
H24 H 0.8239 0.4500 0.1133 0.029 Uiso 1 1 calc R . .
C25 C 0.7662(3) 0.3982(3) 0.2134(2) 0.0206(6) Uani 1 1 d . . .
H25 H 0.8073 0.4545 0.2426 0.025 Uiso 1 1 calc R . .
C26 C 0.6985(3) 0.3184(3) 0.2585(2) 0.0225(7) Uani 1 1 d . . .
H26A H 0.6144 0.3385 0.2518 0.027 Uiso 1 1 calc R . .
H26B H 0.7256 0.3247 0.3149 0.027 Uiso 1 1 calc R . .
C27 C 0.7114(3) 0.1998(3) 0.2330(2) 0.0249(7) Uani 1 1 d . . .
H27A H 0.6958 0.1509 0.2767 0.030 Uiso 1 1 calc R . .
H27B H 0.6522 0.1841 0.1885 0.030 Uiso 1 1 calc R . .
N1 N 1.1367(2) 0.2440(2) 0.29629(15) 0.0168(5) Uani 1 1 d . . .
N2 N 1.1647(2) 0.2207(2) 0.16570(15) 0.0158(5) Uani 1 1 d . . .
Cl1 Cl 1.03057(5) 0.49509(5) 0.21472(4) 0.01078(14) Uani 1 1 d . . .
Rh1 Rh 0.932652(19) 0.318448(19) 0.193664(13) 0.01306(9) Uani 1 1 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
C1 N2 1.351(4) . ?
C1 N1 1.358(4) . ?
C1 Rh1 2.030(3) . ?
C2 C3 1.386(5) . ?
C2 C7 1.390(5) . ?
C2 N1 1.452(4) . ?
C3 C4 1.387(5) . ?
C4 C5 1.377(6) . ?
C5 C6 1.385(6) . ?
C6 C7 1.398(5) . ?
C7 C8 1.503(5) . ?
C9 N1 1.491(4) . ?
C9 C10 1.525(5) . ?
C10 C11 1.528(5) . ?
C11 C12 1.514(4) . ?
C12 N2 1.479(4) . ?
C13 C19 1.391(5) . ?
C13 C14 1.402(4) . ?
C13 N2 1.443(4) . ?
C14 C16 1.395(4) . ?
C14 C15 1.510(5) . ?
C16 C17 1.383(5) . ?
C17 C18 1.384(5) . ?
C18 C19 1.394(5) . ?
C20 C21 1.408(5) . ?
C20 C27 1.519(5) . ?
C20 Rh1 2.120(3) . ?
C21 C22 1.513(5) . ?
C21 Rh1 2.104(3) . ?
C22 C23 1.525(6) . ?
C23 C24 1.515(5) . ?
C24 C25 1.376(5) . ?
C24 Rh1 2.220(3) . ?
C25 C26 1.508(5) . ?
C25 Rh1 2.199(3) . ?
C26 C27 1.528(5) . ?
Cl1 Rh1 2.4470(7) . ?
 
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
N2 C1 N1 117.2(3) . . ?
N2 C1 Rh1 123.7(2) . . ?
N1 C1 Rh1 118.7(2) . . ?
C3 C2 C7 121.3(3) . . ?
C3 C2 N1 119.8(3) . . ?
C7 C2 N1 118.8(3) . . ?
C2 C3 C4 119.6(4) . . ?
C5 C4 C3 120.3(4) . . ?
C4 C5 C6 119.7(3) . . ?
C5 C6 C7 121.3(4) . . ?
C2 C7 C6 117.8(3) . . ?
C2 C7 C8 122.1(3) . . ?
C6 C7 C8 120.1(3) . . ?
N1 C9 C10 112.8(3) . . ?
C9 C10 C11 112.0(3) . . ?
C12 C11 C10 110.3(3) . . ?
N2 C12 C11 112.2(3) . . ?
C19 C13 C14 120.8(3) . . ?
C19 C13 N2 119.4(3) . . ?
C14 C13 N2 119.9(3) . . ?
C16 C14 C13 117.7(3) . . ?
C16 C14 C15 119.2(3) . . ?
C13 C14 C15 123.1(3) . . ?
C17 C16 C14 121.9(3) . . ?
C16 C17 C18 119.7(3) . . ?
C17 C18 C19 119.9(3) . . ?
C13 C19 C18 120.0(3) . . ?
C21 C20 C27 124.3(3) . . ?
C21 C20 Rh1 69.91(18) . . ?
C27 C20 Rh1 113.1(2) . . ?
C20 C21 C22 125.7(3) . . ?
C20 C21 Rh1 71.15(18) . . ?
C22 C21 Rh1 110.0(2) . . ?
C21 C22 C23 113.6(3) . . ?
C24 C23 C22 112.5(3) . . ?
C25 C24 C23 124.9(3) . . ?
C25 C24 Rh1 71.01(19) . . ?
C23 C24 Rh1 110.5(2) . . ?
C24 C25 C26 126.2(3) . . ?
C24 C25 Rh1 72.70(19) . . ?
C26 C25 Rh1 106.8(2) . . ?
C25 C26 C27 113.5(3) . . ?
C20 C27 C26 112.4(3) . . ?
C1 N1 C2 117.1(2) . . ?
C1 N1 C9 128.0(3) . . ?
C2 N1 C9 113.5(2) . . ?
C1 N2 C13 120.5(3) . . ?
C1 N2 C12 123.7(3) . . ?
C13 N2 C12 115.7(2) . . ?
C1 Rh1 C21 94.41(12) . . ?
C1 Rh1 C20 96.89(12) . . ?
C21 Rh1 C20 38.94(13) . . ?
C1 Rh1 C25 158.32(12) . . ?
C21 Rh1 C25 97.93(13) . . ?
C20 Rh1 C25 81.97(12) . . ?
C1 Rh1 C24 164.89(13) . . ?
C21 Rh1 C24 81.70(13) . . ?
C20 Rh1 C24 89.25(13) . . ?
C25 Rh1 C24 36.29(13) . . ?
C1 Rh1 Cl1 86.59(8) . . ?
C21 Rh1 Cl1 157.60(10) . . ?
C20 Rh1 Cl1 163.07(9) . . ?
C25 Rh1 Cl1 88.70(9) . . ?
C24 Rh1 Cl1 91.54(10) . . ?
 
_diffrn_measured_fraction_theta_max    0.998
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.998
_refine_diff_density_max    2.066
_refine_diff_density_min   -0.747
_refine_diff_density_rms    0.120
 
