#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:59:28 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178676 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/87/4078760.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4078760
loop_
_publ_author_name
'Hu, Yue'
'Li, Ling'
'Shaw, Anthony P.'
'Norton, Jack R.'
'Sattler, Wesley'
'Rong, Yi'
_publ_section_title
;
 Synthesis, Electrochemistry, and Reactivity of New Iridium(III) and
 Rhodium(III) Hydrides
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              5058
_journal_paper_doi               10.1021/om300398r
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C21 H24 N Rh'
_chemical_formula_weight         393.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.5040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3812(11)
_cell_length_b                   7.5998(7)
_cell_length_c                   17.7777(15)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.21
_cell_measurement_theta_min      2.38
_cell_volume                     1682.0(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28524
_diffrn_reflns_theta_full        32.74
_diffrn_reflns_theta_max         32.74
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    1.014
_exptl_absorpt_correction_T_max  0.9232
_exptl_absorpt_correction_T_min  0.8464
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.771
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         5939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0337P)²+0.1229P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0782
_reflns_number_gt                4542
_reflns_number_total             5939
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300398r_si_002.cif
_cod_data_source_block           yw2s10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'EMPIRICAL'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4078760
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'
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 0.477708(12) 0.36543(2) 0.169482(10) 0.01512(5) Uani 1 1 d . . .
H1 H 0.509(2) 0.546(4) 0.1513(16) 0.038(8) Uiso 1 1 d . C .
C1 C 0.44834(18) 0.0792(3) 0.13367(14) 0.0204(4) Uani 1 1 d . C .
C2 C 0.53771(18) 0.0889(3) 0.20708(14) 0.0192(4) Uani 1 1 d . C .
C3 C 0.61940(18) 0.1945(3) 0.19343(14) 0.0202(4) Uani 1 1 d . C .
C4 C 0.57983(18) 0.2426(3) 0.10998(14) 0.0214(4) Uani 1 1 d . C .
C5 C 0.47335(18) 0.1769(3) 0.07327(14) 0.0203(4) Uani 1 1 d . C .
C11 C 0.3472(2) -0.0225(3) 0.11904(16) 0.0304(5) Uani 1 1 d . . .
H11A H 0.3526 -0.1375 0.0959 0.046 Uiso 1 1 calc R C .
H11B H 0.2861 0.0425 0.0813 0.046 Uiso 1 1 calc R . .
H11C H 0.3368 -0.0392 0.1703 0.046 Uiso 1 1 calc R . .
C12 C 0.5486(2) 0.0010(3) 0.28492(15) 0.0273(5) Uani 1 1 d . . .
H12A H 0.5840 -0.1133 0.2883 0.041 Uiso 1 1 calc R C .
H12B H 0.4772 -0.0166 0.2872 0.041 Uiso 1 1 calc R . .
H12C H 0.5918 0.0751 0.3303 0.041 Uiso 1 1 calc R . .
C13 C 0.73233(18) 0.2233(3) 0.25247(15) 0.0261(5) Uani 1 1 d . . .
H13A H 0.7810 0.1410 0.2406 0.039 Uiso 1 1 calc R C .
H13B H 0.7350 0.2032 0.3076 0.039 Uiso 1 1 calc R . .
H13C H 0.7545 0.3443 0.2476 0.039 Uiso 1 1 calc R . .
C14 C 0.6445(2) 0.3324(3) 0.06800(16) 0.0283(5) Uani 1 1 d . . .
H14A H 0.6905 0.2459 0.0555 0.042 Uiso 1 1 calc R C .
H14B H 0.6893 0.4239 0.1033 0.042 Uiso 1 1 calc R . .
H14C H 0.5961 0.3861 0.0178 0.042 Uiso 1 1 calc R . .
C15 C 0.4062(2) 0.1815(3) -0.01544(15) 0.0292(5) Uani 1 1 d . . .
H15A H 0.4232 0.0791 -0.0421 0.044 Uiso 1 1 calc R C .
H15B H 0.4217 0.2896 -0.0392 0.044 Uiso 1 1 calc R . .
H15C H 0.3300 0.1789 -0.0229 0.044 Uiso 1 1 calc R . .
C22 C 0.57489(19) 0.4768(3) 0.34713(14) 0.0244(5) Uani 1 1 d . . .
H22 H 0.6392 0.4211 0.3488 0.029 Uiso 1 1 calc R A 1
C23 C 0.5719(2) 0.5551(3) 0.41637(14) 0.0269(5) Uani 1 1 d . C .
H23A H 0.6333 0.5515 0.4650 0.032 Uiso 1 1 calc R . .
C24 C 0.4792(2) 0.6389(3) 0.41499(14) 0.0253(5) Uani 1 1 d . . .
H24A H 0.4767 0.6921 0.4626 0.030 Uiso 1 1 calc R C .
C25 C 0.39085(18) 0.6443(3) 0.34402(13) 0.0209(4) Uani 1 1 d . C .
H25A H 0.3275 0.7035 0.3422 0.025 Uiso 1 1 calc R . .
C26 C 0.39477(17) 0.5626(3) 0.27478(13) 0.0172(4) Uani 1 1 d . . .
C27 C 0.30558(16) 0.5594(3) 0.19747(13) 0.0163(4) Uani 1 1 d . C .
C28 C 0.20663(18) 0.6404(3) 0.18219(14) 0.0203(4) Uani 1 1 d . . .
H28A H 0.1929 0.6998 0.2244 0.024 Uiso 1 1 calc R C .
C29 C 0.12863(18) 0.6342(3) 0.10563(14) 0.0231(4) Uani 1 1 d . C .
H29A H 0.0613 0.6905 0.0947 0.028 Uiso 1 1 calc R . .
C30 C 0.14940(18) 0.5451(3) 0.04481(14) 0.0234(5) Uani 1 1 d . . .
H30A H 0.0963 0.5393 -0.0081 0.028 Uiso 1 1 calc R C .
C31 C 0.24780(17) 0.4651(3) 0.06193(13) 0.0204(4) Uani 1 1 d . C .
H31 H 0.2611 0.4036 0.0200 0.024 Uiso 1 1 calc R B 1
N21 N 0.48696(16) 0.4772(3) 0.27555(12) 0.0177(4) Uani 0.40(2) 1 d P C 1
C32 C 0.32746(15) 0.4709(2) 0.13755(11) 0.0171(4) Uani 0.40(2) 1 d P C 1
C21 C 0.48696(16) 0.4772(3) 0.27555(12) 0.0177(4) Uani 0.60(2) 1 d P C 2
N32 N 0.32746(15) 0.4709(2) 0.13755(11) 0.0171(4) Uani 0.60(2) 1 d P C 2
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'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
H1 Rh1 N21 83.8(10)
H1 Rh1 C32 84.8(10)
N21 Rh1 C32 79.20(8)
H1 Rh1 C3 106.7(10)
N21 Rh1 C3 108.14(8)
C32 Rh1 C3 166.71(8)
H1 Rh1 C5 110.7(10)
N21 Rh1 C5 164.36(8)
C32 Rh1 C5 107.13(8)
C3 Rh1 C5 63.00(8)
H1 Rh1 C4 90.5(11)
N21 Rh1 C4 141.33(8)
C32 Rh1 C4 138.48(8)
C3 Rh1 C4 37.66(8)
C5 Rh1 C4 37.44(8)
H1 Rh1 C1 148.2(11)
N21 Rh1 C1 127.54(8)
C32 Rh1 C1 104.34(8)
C3 Rh1 C1 62.37(8)
C5 Rh1 C1 37.57(8)
C4 Rh1 C1 62.26(8)
H1 Rh1 C2 144.3(10)
N21 Rh1 C2 102.71(8)
C32 Rh1 C2 130.81(7)
C3 Rh1 C2 37.75(8)
C5 Rh1 C2 62.17(8)
C4 Rh1 C2 62.34(8)
C1 Rh1 C2 36.40(8)
C2 C1 C5 108.19(19)
C2 C1 C11 126.4(2)
C5 C1 C11 125.3(2)
C2 C1 Rh1 71.84(12)
C5 C1 Rh1 69.53(12)
C11 C1 Rh1 126.80(16)
C1 C2 C3 108.05(19)
C1 C2 C12 126.5(2)
C3 C2 C12 125.5(2)
C1 C2 Rh1 71.76(12)
C3 C2 Rh1 69.08(12)
C12 C2 Rh1 126.34(15)
C4 C3 C2 107.53(19)
C4 C3 C13 125.6(2)
C2 C3 C13 126.2(2)
C4 C3 Rh1 71.56(12)
C2 C3 Rh1 73.17(12)
C13 C3 Rh1 128.35(16)
C5 C4 C3 108.32(19)
C5 C4 C14 126.6(2)
C3 C4 C14 124.9(2)
C5 C4 Rh1 71.22(12)
C3 C4 Rh1 70.78(12)
C14 C4 Rh1 128.00(15)
C4 C5 C1 107.8(2)
C4 C5 C15 125.9(2)
C1 C5 C15 125.5(2)
C4 C5 Rh1 71.34(12)
C1 C5 Rh1 72.90(12)
C15 C5 Rh1 129.17(15)
N21 C22 C23 121.8(2)
C22 C23 C24 120.0(2)
C25 C24 C23 119.5(2)
C24 C25 C26 119.8(2)
N21 C26 C25 121.3(2)
N21 C26 C27 114.83(18)
C25 C26 C27 123.9(2)
C32 C27 C28 121.36(19)
C32 C27 C26 113.92(18)
C28 C27 C26 124.70(19)
C29 C28 C27 119.9(2)
C28 C29 C30 119.4(2)
C31 C30 C29 119.4(2)
C32 C31 C30 122.4(2)
C22 N21 C26 117.62(19)
C22 N21 Rh1 126.62(16)
C26 N21 Rh1 115.76(14)
C31 C32 C27 117.55(19)
C31 C32 Rh1 126.15(15)
C27 C32 Rh1 116.29(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Rh1 H1 1.51(3)
Rh1 N21 2.030(2)
Rh1 C32 2.0420(19)
Rh1 C3 2.207(2)
Rh1 C5 2.216(2)
Rh1 C4 2.217(2)
Rh1 C1 2.260(2)
Rh1 C2 2.262(2)
C1 C2 1.412(3)
C1 C5 1.442(3)
C1 C11 1.496(3)
C2 C3 1.447(3)
C2 C12 1.495(3)
C3 C4 1.428(3)
C3 C13 1.507(3)
C4 C5 1.423(3)
C4 C14 1.499(3)
C5 C15 1.502(3)
C22 N21 1.381(3)
C22 C23 1.381(3)
C23 C24 1.386(3)
C24 C25 1.378(3)
C25 C26 1.397(3)
C26 N21 1.390(3)
C26 C27 1.453(3)
C27 C32 1.379(3)
C27 C28 1.394(3)
C28 C29 1.379(3)
C29 C30 1.387(3)
C30 C31 1.380(3)
C31 C32 1.377(3)
