data_rob295fi_0m
_audit_creation_date              2013-04-03
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_publ_contact_author_address      ?
_publ_contact_author_email        ?
_publ_contact_author_name         ''
_publ_contact_author_phone        ?
_chemical_name_common             ?
_chemical_name_systematic
;
 ? 
;
_chemical_formula_moiety          'C13 H22 Cl2 N Rh, C H Cl3'
_chemical_formula_sum             'C14 H23 Cl5 N Rh'
_chemical_formula_weight          485.49
_chemical_melting_point           ?
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'
 'Cl' 'Cl' 0.1484 0.1585 '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'
 'Rh' 'Rh' -1.1178 0.9187
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system       'monoclinic'
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 1 21/n 1'
_space_group_name_Hall            '-P 2yn'
loop_
  _space_group_symop_id
  _space_group_symop_operation_xyz
 1 'x, y, z'
 2 '-x+1/2, y+1/2, -z+1/2'
 3 '-x, -y, -z'
 4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                    10.0036(9)
_cell_length_b                    19.0259(18)
_cell_length_c                    10.6590(10)
_cell_angle_alpha                 90.00
_cell_angle_beta                  102.924(4)
_cell_angle_gamma                 90.00
_cell_volume                      1977.3(3)
_cell_formula_units_Z             4
_cell_measurement_reflns_used     6961
_cell_measurement_temperature     120(2)
_cell_measurement_theta_max       30.16
_cell_measurement_theta_min       2.35
_exptl_absorpt_coefficient_mu     1.532
_exptl_absorpt_correction_T_max   0.7461
_exptl_absorpt_correction_T_min   0.7168
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0414 before and 0.0371 after correction.
The Ratio of minimum to maximum transmission is 0.9607.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour             ?
_exptl_crystal_density_diffrn     1.631
_exptl_crystal_density_meas       .
_exptl_crystal_density_method     'not measured'
_exptl_crystal_description        block
_exptl_crystal_F_000              976
_exptl_crystal_size_max           0.31
_exptl_crystal_size_mid           0.28
_exptl_crystal_size_min           0.2
_exptl_special_details
;
 ? 
;
_diffrn_reflns_av_R_equivalents   0.0251
_diffrn_reflns_av_unetI/netI      0.0315
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_k_max        26
_diffrn_reflns_limit_k_min        -23
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_limit_l_min        -14
_diffrn_reflns_number             17409
_diffrn_reflns_theta_full         30.24
_diffrn_reflns_theta_max          30.24
_diffrn_reflns_theta_min          2.52
_diffrn_ambient_temperature       120(2)
_diffrn_detector_area_resol_mean  ?
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        '\f and \w scans'
_diffrn_radiation_monochromator   'graphite'
_diffrn_radiation_type            'MoK\a'
_diffrn_radiation_wavelength      0.71073
_diffrn_source                    'fine-focus sealed tube'
_diffrn_standards_decay_%         ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_number          0
_reflns_number_gt                 5090
_reflns_number_total              5810
_reflns_threshold_expression      >2sigma(I)
_computing_cell_refinement        ?
_computing_data_collection        ?
_computing_data_reduction         'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_refine_diff_density_max          0.494
_refine_diff_density_min          -0.465
_refine_diff_density_rms          0.080
_refine_ls_extinction_coef        ?
_refine_ls_extinction_method      none
_refine_ls_goodness_of_fit_ref    1.027
_refine_ls_hydrogen_treatment     riding
_refine_ls_matrix_type            full
_refine_ls_number_parameters      195
_refine_ls_number_reflns          5810
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0325
_refine_ls_R_factor_gt            0.0267
_refine_ls_restrained_S_all       1.027
_refine_ls_shift/su_max           0.004
_refine_ls_shift/su_mean          0.000
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0172P)^2^+0.9426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme       calc
_refine_ls_wR_factor_gt           0.0504
_refine_ls_wR_factor_ref          0.0524
_refine_special_details
;
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H3A,H3B} of C3, H14 of C14, {H2A,H2B} of C2, H1 of N1, {H4A,H4B} of C4
 At 1.5 times of:
  {H11A,H11B,H11C} of C11, {H12A,H12B,H12C} of C12, {H13A,H13B,H13C} of C13,
  {H10A,H10B,H10C} of C10, {H1A,H1B,H1C} of C1
2.a Ternary CH refined with riding coordinates:
 N1(H1), C14(H14)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C3(H3A,H3B)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C1(H1A,H1B,H1C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C12(H12A,H12B,H12C)
;
_atom_sites_solution_hydrogens    geom
_atom_sites_solution_primary      iterative
_atom_sites_solution_secondary    difmap
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 0.704252(13) 0.394676(7) 0.409018(12) 0.01436(4) Uani 1 1 d . . .
 Cl1 Cl 0.71317(4) 0.49092(2) 0.56397(4) 0.02167(9) Uani 1 1 d . . .
 Cl2 Cl 0.81856(5) 0.31507(3) 0.58001(4) 0.03132(12) Uani 1 1 d . . .
 Cl5 Cl 0.71011(5) 0.33120(3) -0.08882(5) 0.03485(12) Uani 1 1 d . . .
 Cl4 Cl 1.00665(5) 0.35606(3) -0.04299(6) 0.03696(13) Uani 1 1 d . . .
 Cl3 Cl 0.81799(6) 0.47465(3) -0.05862(5) 0.03706(13) Uani 1 1 d . . .
 N1 N 0.50401(15) 0.37508(8) 0.44886(15) 0.0196(3) Uani 1 1 d . . .
 H1 H 0.4642 0.4194 0.4468 0.023 Uiso 1 1 calc R . .
 C2 C 0.40550(18) 0.33378(10) 0.34955(19) 0.0237(4) Uani 1 1 d . . .
 H2A H 0.3183 0.3285 0.3780 0.028 Uiso 1 1 calc R . .
 H2B H 0.4436 0.2862 0.3438 0.028 Uiso 1 1 calc R . .
 C5 C 0.63048(18) 0.37897(9) 0.20446(16) 0.0189(4) Uani 1 1 d . . .
 C4 C 0.48779(18) 0.35445(10) 0.13901(18) 0.0235(4) Uani 1 1 d . . .
 H4A H 0.4916 0.3035 0.1216 0.028 Uiso 1 1 calc R . .
 H4B H 0.4603 0.3786 0.0549 0.028 Uiso 1 1 calc R . .
 C8 C 0.82083(18) 0.45125(10) 0.28732(17) 0.0214(4) Uani 1 1 d . . .
 C6 C 0.74768(18) 0.33415(10) 0.25264(17) 0.0211(4) Uani 1 1 d . . .
 C14 C 0.8408(2) 0.38915(10) -0.11779(19) 0.0262(4) Uani 1 1 d . . .
 H14 H 0.8337 0.3922 -0.2127 0.031 Uiso 1 1 calc R . .
 C7 C 0.86638(18) 0.37996(11) 0.30134(18) 0.0235(4) Uani 1 1 d . . .
 C3 C 0.37506(18) 0.36727(10) 0.21557(19) 0.0251(4) Uani 1 1 d . . .
 H3A H 0.3636 0.4186 0.2248 0.030 Uiso 1 1 calc R . .
 H3B H 0.2871 0.3484 0.1653 0.030 Uiso 1 1 calc R . .
 C9 C 0.67307(18) 0.45153(10) 0.22978(16) 0.0185(3) Uani 1 1 d . . .
 C10 C 0.7520(2) 0.25479(11) 0.2464(2) 0.0315(5) Uani 1 1 d . . .
 H10A H 0.8128 0.2366 0.3248 0.047 Uiso 1 1 calc R . .
 H10B H 0.7866 0.2404 0.1712 0.047 Uiso 1 1 calc R . .
 H10C H 0.6595 0.2359 0.2391 0.047 Uiso 1 1 calc R . .
 C1 C 0.5032(2) 0.34746(11) 0.57998(19) 0.0301(5) Uani 1 1 d . . .
 H1A H 0.5346 0.2985 0.5867 0.045 Uiso 1 1 calc R . .
 H1B H 0.4099 0.3498 0.5942 0.045 Uiso 1 1 calc R . .
 H1C H 0.5646 0.3759 0.6450 0.045 Uiso 1 1 calc R . .
 C11 C 1.01220(19) 0.35443(13) 0.3528(2) 0.0342(5) Uani 1 1 d . . .
 H11A H 1.0713 0.3946 0.3852 0.051 Uiso 1 1 calc R . .
 H11B H 1.0456 0.3314 0.2835 0.051 Uiso 1 1 calc R . .
 H11C H 1.0137 0.3209 0.4229 0.051 Uiso 1 1 calc R . .
 C13 C 0.5879(2) 0.51672(10) 0.18978(19) 0.0269(4) Uani 1 1 d . . .
 H13A H 0.4906 0.5054 0.1805 0.040 Uiso 1 1 calc R . .
 H13B H 0.6032 0.5338 0.1074 0.040 Uiso 1 1 calc R . .
 H13C H 0.6145 0.5532 0.2555 0.040 Uiso 1 1 calc R . .
 C12 C 0.9053(2) 0.51726(11) 0.3212(2) 0.0310(5) Uani 1 1 d . . .
 H12A H 0.8587 0.5490 0.3700 0.046 Uiso 1 1 calc R . .
 H12B H 0.9160 0.5406 0.2421 0.046 Uiso 1 1 calc R . .
 H12C H 0.9958 0.5049 0.3736 0.046 Uiso 1 1 calc R . .

loop_
  _atom_site_aniso_label
  _atom_site_aniso_U_11
  _atom_site_aniso_U_22
  _atom_site_aniso_U_33
  _atom_site_aniso_U_23
  _atom_site_aniso_U_13
  _atom_site_aniso_U_12
 Rh1 0.01415(6) 0.01495(7) 0.01434(7) 0.00077(5) 0.00395(5) 0.00295(5)
 Cl1 0.0186(2) 0.0217(2) 0.0245(2) -0.00673(17) 0.00444(16) 0.00104(17)
 Cl2 0.0420(3) 0.0317(3) 0.0205(2) 0.00696(19) 0.0075(2) 0.0215(2)
 Cl5 0.0361(3) 0.0411(3) 0.0295(3) 0.0002(2) 0.0117(2) -0.0065(2)
 Cl4 0.0315(3) 0.0264(3) 0.0486(3) -0.0005(2) -0.0003(2) 0.0035(2)
 Cl3 0.0428(3) 0.0280(3) 0.0373(3) -0.0049(2) 0.0026(2) 0.0082(2)
 N1 0.0200(7) 0.0165(8) 0.0241(8) -0.0003(6) 0.0090(6) 0.0005(6)
 C2 0.0197(9) 0.0190(10) 0.0340(11) -0.0020(8) 0.0094(8) -0.0040(7)
 C5 0.0216(8) 0.0203(9) 0.0154(8) -0.0010(7) 0.0057(7) -0.0004(7)
 C4 0.0247(9) 0.0229(10) 0.0207(9) -0.0024(7) 0.0006(7) -0.0031(8)
 C8 0.0196(8) 0.0288(10) 0.0171(9) 0.0020(7) 0.0066(7) -0.0038(7)
 C6 0.0248(9) 0.0235(10) 0.0171(9) -0.0020(7) 0.0088(7) 0.0040(7)
 C14 0.0299(10) 0.0252(11) 0.0230(10) -0.0014(8) 0.0044(8) 0.0005(8)
 C7 0.0183(8) 0.0343(11) 0.0194(9) 0.0000(8) 0.0077(7) 0.0034(8)
 C3 0.0173(8) 0.0220(10) 0.0328(11) -0.0036(8) -0.0010(7) -0.0001(7)
 C9 0.0202(8) 0.0205(9) 0.0145(8) 0.0027(7) 0.0031(6) -0.0010(7)
 C10 0.0410(12) 0.0250(11) 0.0308(11) -0.0038(9) 0.0131(9) 0.0108(9)
 C1 0.0360(11) 0.0300(11) 0.0290(11) 0.0027(9) 0.0175(9) -0.0028(9)
 C11 0.0205(9) 0.0467(14) 0.0369(12) -0.0016(10) 0.0097(9) 0.0097(9)
 C13 0.0327(10) 0.0213(10) 0.0236(10) 0.0054(8) -0.0007(8) 0.0006(8)
 C12 0.0257(10) 0.0377(12) 0.0286(11) 0.0025(9) 0.0041(8) -0.0105(9)

_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 Cl1 2.4543(5) . ?
 Rh1 Cl2 2.4477(5) . ?
 Rh1 N1 2.1708(14) . ?
 Rh1 C5 2.1606(18) . ?
 Rh1 C8 2.2086(16) . ?
 Rh1 C6 2.1488(17) . ?
 Rh1 C7 2.2043(16) . ?
 Rh1 C9 2.1566(17) . ?
 Cl5 C14 1.789(2) . ?
 Cl4 C14 1.787(2) . ?
 Cl3 C14 1.778(2) . ?
 N1 C2 1.497(2) . ?
 N1 C1 1.495(2) . ?
 C2 C3 1.531(3) . ?
 C5 C4 1.515(2) . ?
 C5 C6 1.448(2) . ?
 C5 C9 1.452(3) . ?
 C4 C3 1.552(2) . ?
 C8 C7 1.428(3) . ?
 C8 C9 1.468(3) . ?
 C8 C12 1.512(3) . ?
 C6 C7 1.471(3) . ?
 C6 C10 1.512(3) . ?
 C7 C11 1.519(3) . ?
 C9 C13 1.511(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
 Cl2 Rh1 Cl1 91.144(18) . . ?
 N1 Rh1 Cl1 83.84(4) . . ?
 N1 Rh1 Cl2 92.63(4) . . ?
 N1 Rh1 C8 146.11(6) . . ?
 N1 Rh1 C7 153.98(7) . . ?
 C5 Rh1 Cl1 137.32(5) . . ?
 C5 Rh1 Cl2 131.53(5) . . ?
 C5 Rh1 N1 92.97(6) . . ?
 C5 Rh1 C8 65.21(7) . . ?
 C5 Rh1 C7 65.29(7) . . ?
 C8 Rh1 Cl1 95.00(5) . . ?
 C8 Rh1 Cl2 121.25(5) . . ?
 C6 Rh1 Cl1 159.83(5) . . ?
 C6 Rh1 Cl2 95.98(5) . . ?
 C6 Rh1 N1 114.53(6) . . ?
 C6 Rh1 C5 39.26(7) . . ?
 C6 Rh1 C8 65.21(7) . . ?
 C6 Rh1 C7 39.47(7) . . ?
 C6 Rh1 C9 66.16(7) . . ?
 C7 Rh1 Cl1 121.66(5) . . ?
 C7 Rh1 Cl2 91.92(5) . . ?
 C7 Rh1 C8 37.76(7) . . ?
 C9 Rh1 Cl1 101.43(5) . . ?
 C9 Rh1 Cl2 157.06(5) . . ?
 C9 Rh1 N1 107.61(6) . . ?
 C9 Rh1 C5 39.31(7) . . ?
 C9 Rh1 C8 39.28(7) . . ?
 C9 Rh1 C7 65.16(7) . . ?
 C2 N1 Rh1 116.23(10) . . ?
 C1 N1 Rh1 116.20(12) . . ?
 C1 N1 C2 109.64(14) . . ?
 N1 C2 C3 113.78(15) . . ?
 C4 C5 Rh1 125.53(11) . . ?
 C6 C5 Rh1 69.93(10) . . ?
 C6 C5 C4 125.92(16) . . ?
 C6 C5 C9 108.26(16) . . ?
 C9 C5 Rh1 70.20(10) . . ?
 C9 C5 C4 125.81(16) . . ?
 C5 C4 C3 115.47(15) . . ?
 C7 C8 Rh1 70.96(10) . . ?
 C7 C8 C9 108.37(16) . . ?
 C7 C8 C12 128.02(17) . . ?
 C9 C8 Rh1 68.45(9) . . ?
 C9 C8 C12 123.60(17) . . ?
 C12 C8 Rh1 127.20(13) . . ?
 C5 C6 Rh1 70.81(9) . . ?
 C5 C6 C7 107.58(16) . . ?
 C5 C6 C10 126.96(18) . . ?
 C7 C6 Rh1 72.30(10) . . ?
 C7 C6 C10 125.33(17) . . ?
 C10 C6 Rh1 125.59(13) . . ?
 Cl4 C14 Cl5 110.32(11) . . ?
 Cl3 C14 Cl5 110.25(10) . . ?
 Cl3 C14 Cl4 110.12(11) . . ?
 C8 C7 Rh1 71.28(9) . . ?
 C8 C7 C6 108.20(16) . . ?
 C8 C7 C11 126.85(18) . . ?
 C6 C7 Rh1 68.23(9) . . ?
 C6 C7 C11 124.91(18) . . ?
 C11 C7 Rh1 127.72(13) . . ?
 C2 C3 C4 114.13(15) . . ?
 C5 C9 Rh1 70.49(10) . . ?
 C5 C9 C8 107.47(16) . . ?
 C5 C9 C13 127.17(16) . . ?
 C8 C9 Rh1 72.27(10) . . ?
 C8 C9 C13 124.92(17) . . ?
 C13 C9 Rh1 128.48(12) . . ?