#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:44:30 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179075 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/37/4303708.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_4303708
loop_
_publ_author_name
'Arup Sinha'
'S. M. Wahidur Rahaman'
'Mithun Sarkar'
'Biswajit Saha'
'Prosenjit Daw'
'Jitendra K. Bera'
_publ_contact_author_address
'Department of Chemistry, IIT Kanpur, Kanpur 208016, INDIA.'
_publ_contact_author_email       jbera@iitk.ac.in
_publ_contact_author_fax         '+ 91-512-2597436'
_publ_contact_author_name        'Jitendra K. Bera'
_publ_contact_author_phone       '+ 91-512-2597336'
_publ_section_title
;
Multifaceted Coordination of Naphthyridine-Functionalized N-Heterocyclic
Carbene: A Novel "IrIII(CN)(CC)" Compound and Its Evaluation as
Transfer Hydrogenation Catalyst
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11114
_journal_page_last               11122
_journal_paper_doi               10.1021/ic901502n
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C28 H30 Br N4 Rh'
_chemical_formula_sum            'C28 H30 Br N4 Rh'
_chemical_formula_weight         605.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.294(3)
_cell_angle_beta                 94.061(3)
_cell_angle_gamma                103.084(3)
_cell_formula_units_Z            2
_cell_length_a                   6.9091(13)
_cell_length_b                   12.842(3)
_cell_length_c                   14.458(3)
_cell_measurement_temperature    100(2)
_cell_volume                     1221.1(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP
_computing_publication_material  ciftab
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       'omega 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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0558
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10451
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    2.360
_exptl_absorpt_correction_T_max  0.6012
_exptl_absorpt_correction_T_min  0.5282
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         2.223
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5687
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0482
_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)+(0.0783P)²+0.7896P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1345
_reflns_number_gt                4574
_reflns_number_total             5687
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901502n_si_002_4.cif
_cod_data_source_block           complound3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4303708
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.43881(5) 0.30527(2) 0.72282(2) 0.01305(11) Uani 1 1 d . . .
Br1 Br 0.76546(6) 0.33184(4) 0.81957(3) 0.02176(13) Uani 1 1 d . . .
C6 C 0.1494(6) 0.2394(4) 0.6454(3) 0.0185(9) Uani 1 1 d . . .
H6 H 0.0384 0.2292 0.6862 0.022 Uiso 1 1 calc R . .
N2 N 0.2468(5) 0.2262(3) 1.0233(2) 0.0136(7) Uani 1 1 d . . .
C21 C 0.2277(6) 0.4239(3) 0.9830(3) 0.0151(8) Uani 1 1 d . . .
H21 H 0.1769 0.4172 1.0416 0.018 Uiso 1 1 calc R . .
N1 N 0.2304(5) 0.1255(3) 1.1403(3) 0.0152(7) Uani 1 1 d . . .
C20 C 0.2571(6) 0.2338(3) 0.9340(3) 0.0132(8) Uani 1 1 d . . .
C13 C 0.2380(6) -0.0645(3) 1.1032(3) 0.0171(8) Uani 1 1 d . . .
H13 H 0.2379 -0.1292 1.1264 0.021 Uiso 1 1 calc R . .
N4 N 0.3413(5) 0.4873(3) 0.8608(2) 0.0143(7) Uani 1 1 d . . .
C16 C 0.2454(6) 0.0344(3) 0.9778(3) 0.0135(8) Uani 1 1 d . . .
C23 C 0.3395(6) 0.3798(3) 0.8399(3) 0.0131(8) Uani 1 1 d . . .
C24 C 0.4305(6) 0.5662(3) 0.8055(3) 0.0160(8) Uani 1 1 d . . .
H24A H 0.4946 0.5288 0.7549 0.019 Uiso 1 1 calc R . .
H24B H 0.5373 0.6234 0.8473 0.019 Uiso 1 1 calc R . .
N3 N 0.2688(5) 0.3406(3) 0.9165(2) 0.0142(7) Uani 1 1 d . . .
C22 C 0.2742(6) 0.5151(3) 0.9477(3) 0.0158(8) Uani 1 1 d . . .
H22 H 0.2632 0.5856 0.9770 0.019 Uiso 1 1 calc R . .
C12 C 0.2326(6) 0.0326(4) 1.1669(3) 0.0163(8) Uani 1 1 d . . .
C15 C 0.2459(7) -0.1671(3) 0.9399(3) 0.0191(9) Uani 1 1 d . . .
H15A H 0.2458 -0.2268 0.9737 0.029 Uiso 1 1 calc R . .
H15B H 0.3666 -0.1541 0.9076 0.029 Uiso 1 1 calc R . .
H15C H 0.1272 -0.1868 0.8932 0.029 Uiso 1 1 calc R . .
C18 C 0.2538(6) 0.0476(3) 0.8833(3) 0.0143(8) Uani 1 1 d . . .
H18 H 0.2552 -0.0132 0.8353 0.017 Uiso 1 1 calc R . .
C1 C 0.5169(7) 0.1842(4) 0.6143(3) 0.0229(10) Uani 1 1 d . . .
H1 H 0.6321 0.1557 0.6357 0.027 Uiso 1 1 calc R . .
C25 C 0.2876(6) 0.6207(3) 0.7608(3) 0.0151(8) Uani 1 1 d . . .
C17 C 0.2395(6) 0.1278(3) 1.0467(3) 0.0122(8) Uani 1 1 d . . .
C14 C 0.2433(6) -0.0652(3) 1.0093(3) 0.0148(8) Uani 1 1 d . . .
C29 C 0.2475(7) 0.7600(4) 0.6738(3) 0.0251(10) Uani 1 1 d . . .
H29 H 0.3052 0.8181 0.6442 0.030 Uiso 1 1 calc R . .
C11 C 0.2229(7) 0.0295(4) 1.2697(3) 0.0231(10) Uani 1 1 d . . .
H11A H 0.2076 0.0998 1.3036 0.035 Uiso 1 1 calc R . .
H11B H 0.3465 0.0151 1.2962 0.035 Uiso 1 1 calc R . .
H11C H 0.1084 -0.0286 1.2763 0.035 Uiso 1 1 calc R . .
C30 C 0.3695(7) 0.7079(4) 0.7184(3) 0.0191(9) Uani 1 1 d . . .
H30 H 0.5106 0.7316 0.7203 0.023 Uiso 1 1 calc R . .
C26 C 0.0807(6) 0.5887(4) 0.7573(3) 0.0184(9) Uani 1 1 d . . .
H26 H 0.0224 0.5290 0.7850 0.022 Uiso 1 1 calc R . .
C19 C 0.2601(6) 0.1464(3) 0.8598(3) 0.0153(8) Uani 1 1 d . . .
H19 H 0.2661 0.1560 0.7964 0.018 Uiso 1 1 calc R . .
C5 C 0.2216(7) 0.3474(4) 0.6362(3) 0.0222(9) Uani 1 1 d . . .
H5 H 0.1515 0.3994 0.6716 0.027 Uiso 1 1 calc R . .
C28 C 0.0416(8) 0.7282(4) 0.6719(4) 0.0264(10) Uani 1 1 d . . .
H28 H -0.0419 0.7648 0.6419 0.032 Uiso 1 1 calc R . .
C3 C 0.4544(8) 0.3183(4) 0.5117(3) 0.0298(11) Uani 1 1 d . . .
H3A H 0.3766 0.2526 0.4662 0.036 Uiso 1 1 calc R . .
H3B H 0.5486 0.3624 0.4769 0.036 Uiso 1 1 calc R . .
C27 C -0.0421(7) 0.6420(4) 0.7144(4) 0.0254(10) Uani 1 1 d . . .
H27 H -0.1831 0.6198 0.7139 0.030 Uiso 1 1 calc R . .
C7 C 0.1406(7) 0.1401(4) 0.5683(3) 0.0229(10) Uani 1 1 d . . .
H7A H 0.1213 0.1597 0.5057 0.028 Uiso 1 1 calc R . .
H7B H 0.0232 0.0815 0.5732 0.028 Uiso 1 1 calc R . .
C4 C 0.3115(8) 0.3850(4) 0.5522(3) 0.0293(11) Uani 1 1 d . . .
H4A H 0.3848 0.4626 0.5714 0.035 Uiso 1 1 calc R . .
H4B H 0.2024 0.3797 0.5021 0.035 Uiso 1 1 calc R . .
C8 C 0.3287(7) 0.0962(4) 0.5739(3) 0.0253(10) Uani 1 1 d . . .
H8A H 0.3098 0.0403 0.6137 0.030 Uiso 1 1 calc R . .
H8B H 0.3462 0.0601 0.5096 0.030 Uiso 1 1 calc R . .
C2 C 0.5719(7) 0.2836(4) 0.5877(3) 0.0242(10) Uani 1 1 d . . .
H2 H 0.7197 0.3148 0.5939 0.029 Uiso 1 1 calc R . .
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'
Br Br -0.2901 2.4595 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C23 Rh1 C5 89.90(17) . . ?
C23 Rh1 C6 95.27(16) . . ?
C5 Rh1 C6 38.42(18) . . ?
C23 Rh1 C1 163.68(17) . . ?
C5 Rh1 C1 97.41(18) . . ?
C6 Rh1 C1 81.82(17) . . ?
C23 Rh1 C2 159.89(17) . . ?
C5 Rh1 C2 81.29(18) . . ?
C6 Rh1 C2 89.03(18) . . ?
C1 Rh1 C2 36.43(17) . . ?
C23 Rh1 H19 74.6 . . ?
C5 Rh1 H19 108.0 . . ?
C6 Rh1 H19 72.9 . . ?
C1 Rh1 H19 89.3 . . ?
C2 Rh1 H19 125.3 . . ?
C23 Rh1 Br1 88.14(11) . . ?
C5 Rh1 Br1 156.61(13) . . ?
C6 Rh1 Br1 164.86(13) . . ?
C1 Rh1 Br1 90.77(13) . . ?
C2 Rh1 Br1 92.82(13) . . ?
H19 Rh1 Br1 94.0 . . ?
C5 C6 C7 124.5(4) . . ?
C5 C6 Rh1 70.0(3) . . ?
C7 C6 Rh1 113.1(3) . . ?
C20 N2 C17 118.2(4) . . ?
C22 C21 N3 106.5(4) . . ?
C12 N1 C17 117.4(4) . . ?
N2 C20 C19 124.8(4) . . ?
N2 C20 N3 114.3(4) . . ?
C19 C20 N3 121.0(4) . . ?
C14 C13 C12 120.4(4) . . ?
C23 N4 C22 111.6(3) . . ?
C23 N4 C24 123.8(3) . . ?
C22 N4 C24 124.0(3) . . ?
C18 C16 C17 117.2(4) . . ?
C18 C16 C14 124.9(4) . . ?
C17 C16 C14 118.0(4) . . ?
N4 C23 N3 104.0(3) . . ?
N4 C23 Rh1 124.9(3) . . ?
N3 C23 Rh1 131.0(3) . . ?
N4 C24 C25 115.2(3) . . ?
C23 N3 C21 110.8(3) . . ?
C23 N3 C20 126.4(3) . . ?
C21 N3 C20 122.5(3) . . ?
C21 C22 N4 107.2(4) . . ?
N1 C12 C13 123.5(4) . . ?
N1 C12 C11 117.7(4) . . ?
C13 C12 C11 118.7(4) . . ?
C19 C18 C16 121.0(4) . . ?
C2 C1 C8 125.1(5) . . ?
C2 C1 Rh1 72.8(3) . . ?
C8 C1 Rh1 108.5(3) . . ?
C26 C25 C30 118.1(4) . . ?
C26 C25 C24 124.4(4) . . ?
C30 C25 C24 117.5(4) . . ?
N2 C17 N1 115.3(4) . . ?
N2 C17 C16 121.8(4) . . ?
N1 C17 C16 122.8(4) . . ?
C13 C14 C16 117.9(4) . . ?
C13 C14 C15 121.6(4) . . ?
C16 C14 C15 120.5(4) . . ?
C30 C29 C28 120.5(4) . . ?
C29 C30 C25 120.8(4) . . ?
C27 C26 C25 121.4(4) . . ?
C18 C19 C20 117.1(4) . . ?
C6 C5 C4 126.4(4) . . ?
C6 C5 Rh1 71.6(3) . . ?
C4 C5 Rh1 110.0(3) . . ?
C29 C28 C27 119.4(4) . . ?
C2 C3 C4 112.3(4) . . ?
C26 C27 C28 119.8(4) . . ?
C6 C7 C8 113.4(4) . . ?
C5 C4 C3 112.9(4) . . ?
C1 C8 C7 113.2(4) . . ?
C1 C2 C3 124.2(5) . . ?
C1 C2 Rh1 70.7(3) . . ?
C3 C2 Rh1 110.9(3) . . ?
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 C23 2.033(4) . ?
Rh1 C5 2.111(5) . ?
Rh1 C6 2.132(4) . ?
Rh1 C1 2.191(4) . ?
Rh1 C2 2.217(4) . ?
Rh1 H19 2.4701 . ?
Rh1 Br1 2.4900(7) . ?
C6 C5 1.396(6) . ?
C6 C7 1.524(6) . ?
N2 C20 1.319(5) . ?
N2 C17 1.356(5) . ?
C21 C22 1.343(6) . ?
C21 N3 1.400(5) . ?
N1 C12 1.321(5) . ?
N1 C17 1.365(5) . ?
C20 C19 1.411(6) . ?
C20 N3 1.424(5) . ?
C13 C14 1.359(6) . ?
C13 C12 1.421(6) . ?
N4 C23 1.356(5) . ?
N4 C22 1.386(5) . ?
N4 C24 1.456(5) . ?
C16 C18 1.410(6) . ?
C16 C17 1.426(6) . ?
C16 C14 1.430(6) . ?
C23 N3 1.372(5) . ?
C24 C25 1.505(6) . ?
C12 C11 1.499(6) . ?
C15 C14 1.504(6) . ?
C18 C19 1.363(6) . ?
C1 C2 1.378(7) . ?
C1 C8 1.517(7) . ?
C25 C26 1.390(6) . ?
C25 C30 1.400(6) . ?
C29 C30 1.381(7) . ?
C29 C28 1.385(7) . ?
C26 C27 1.383(6) . ?
C5 C4 1.509(7) . ?
C28 C27 1.394(7) . ?
C3 C2 1.509(7) . ?
C3 C4 1.528(7) . ?
C7 C8 1.531(7) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rh1 C23 C19 H19 -24.4 . . . . ?
