#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/00/2010039.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2010039
loop_
_publ_author_name
'Flörke, Ulrich'
'Haupt, Hans-Jürgen'
_publ_section_title
;
 Rhodium(I) complexes with 1,5-diazabicyclo[4.3.0]non-5-ene (dbn) as a
 ligand: [RhCl(nbd)(dbn)] (I) and [Rh(dbn)₂(cod)][PF₆] (II) (nbd =
 norbornadiene, cod = 1,5-cyclooctadiene)
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1424
_journal_page_last               1427
_journal_paper_doi               10.1107/S0108270194003823
_journal_volume                  50
_journal_year                    1994
_chemical_formula_moiety         '[Rh1 (C7 H12 N2)2 (C8 H12)] [P1 F6]'
_chemical_formula_sum            'C22 H36 F6 N4 P Rh'
_chemical_formula_weight         604.43
_chemical_name_systematic
;
 bis(diazabicyclo[4.3.0]non-5-ene)(cycloocta-1,5-diene)rhodium(I)hexa-
 fluorophosphate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 94.920(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.245(3)
_cell_length_b                   8.3330(10)
_cell_length_c                   16.535(3)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      7.5
_cell_volume                     2504.6(7)
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3m/V'
_diffrn_measurement_method       ω-2θ
_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  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5756
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.809
_exptl_absorpt_correction_T_max  0.451
_exptl_absorpt_correction_T_min  0.398
_exptl_absorpt_correction_type   'empirical via \y-scans'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_description       prism
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.380
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.037
_refine_ls_goodness_of_fit_obs   1.046
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_restrained_S_obs      1.046
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_obs          0.0347
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; w = 1/[\s^2^(F~o~^2^) + (0.0524P)^2^ + 2.3655P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.0967
_refine_ls_wR_factor_obs         0.0904
_reflns_number_observed          2495
_reflns_number_total             2883
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            hr1015.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2010039
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y, -z-1/2'
'-x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
Rh1 0.0000 0.13238(3) 0.2500 0.04222(12) Uani d S 1 . Rh
N1 -0.08157(12) -0.0477(3) 0.2250(2) 0.0477(5) Uani d . 1 . N
N2 -0.14580(13) -0.2118(3) 0.12792(15) 0.0490(6) Uani d . 1 . N
C1 -0.1343(2) -0.0959(5) 0.2825(2) 0.0653(9) Uani d . 1 . C
H1A -0.1143(2) -0.1867(5) 0.3138(2) 0.080 Uiso calc R 1 1 H
H1B -0.1399(2) -0.0082(5) 0.3201(2) 0.080 Uiso calc R 1 1 H
C21 -0.2066(4) -0.1394(17) 0.2445(5) 0.066(2) Uani d P 0.73(3) 1 C
H21A -0.2319(4) -0.0421(17) 0.2257(5) 0.080 Uiso calc PR 0.73(3) 1 H
H21B -0.2349(4) -0.1871(17) 0.2854(5) 0.080 Uiso calc PR 0.73(3) 1 H
C22 -0.1882(12) -0.221(4) 0.2586(11) 0.065(5) Uani d P 0.27(3) 2 C
H22A -0.1706(12) -0.320(4) 0.2838(11) 0.080 Uiso calc PR 0.27(3) 2 H
H22B -0.2335(12) -0.193(4) 0.2821(11) 0.080 Uiso calc PR 0.27(3) 2 H
C3 -0.2060(2) -0.2520(5) 0.1756(2) 0.0761(12) Uani d . 1 . C
H3A -0.2003(2) -0.3610(5) 0.1956(2) 0.080 Uiso calc R 1 1 H
H3B -0.2522(2) -0.2451(5) 0.1421(2) 0.080 Uiso calc R 1 1 H
C4 -0.1481(2) -0.2445(5) 0.0414(2) 0.0623(8) Uani d . 1 . C
H4A -0.1874(2) -0.1848(5) 0.0118(2) 0.080 Uiso calc R 1 . H
H4B -0.1551(2) -0.3581(5) 0.0304(2) 0.080 Uiso calc R 1 . H
C5 -0.0744(2) -0.1894(6) 0.0190(2) 0.0780(11) Uani d . 1 . C
H5A -0.0408(2) -0.2795(6) 0.0177(2) 0.080 Uiso calc R 1 . H
H5B -0.0787(2) -0.1384(6) -0.0339(2) 0.080 Uiso calc R 1 . H
C6 -0.0473(2) -0.0721(5) 0.0834(2) 0.0633(9) Uani d . 1 . C
H6A -0.0552(2) 0.0374(5) 0.0647(2) 0.080 Uiso calc R 1 . H
H6B 0.0047(2) -0.0876(5) 0.0990(2) 0.080 Uiso calc R 1 . H
C7 -0.09274(15) -0.1087(3) 0.1536(2) 0.0448(6) Uani d . 1 . C
C8 0.0417(3) 0.4474(5) 0.1726(3) 0.099(2) Uani d . 1 . C
H8A 0.0702(3) 0.4647(5) 0.1272(3) 0.080 Uiso d R 1 . H
H8B 0.0431(3) 0.5447(5) 0.2039(3) 0.080 Uiso d R 1 . H
C9 0.0783(2) 0.3128(5) 0.2255(3) 0.0710(10) Uani d . 1 . C
H9 0.1041(2) 0.2339(5) 0.2001(3) 0.080 Uiso d R 1 . H
C10 0.0746(2) 0.3018(4) 0.3070(3) 0.0709(10) Uani d . 1 . C
H10 0.0983(2) 0.2150(4) 0.3331(3) 0.080 Uiso d R 1 . H
C11 0.0355(3) 0.4152(6) 0.3574(3) 0.0931(14) Uani d . 1 . C
H11A 0.0622(3) 0.5146(6) 0.3610(3) 0.080 Uiso d R 1 . H
H11B 0.0361(3) 0.3716(6) 0.4112(3) 0.080 Uiso d R 1 . H
P1 0.2500 0.2500 0.5000 0.0619(3) Uani d S 1 . P
F1 0.3331(2) 0.2424(6) 0.4860(2) 0.1489(15) Uani d . 1 . F
F2 0.2606(2) 0.1064(3) 0.5619(2) 0.1218(12) Uani d . 1 . F
F3 0.2330(2) 0.1307(3) 0.4275(2) 0.1227(13) Uani d . 1 . F
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'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C10 Rh1 C10 6_556 . 96.7(2) n
C10 Rh1 N1 6_556 . 88.39(13) n
C10 Rh1 N1 . . 164.81(13) n
C10 Rh1 N1 6_556 6_556 164.81(14) n
C10 Rh1 N1 . 6_556 88.39(13) n
N1 Rh1 N1 . 6_556 90.40(10) y
C10 Rh1 C9 6_556 6_556 37.2(2) n
C10 Rh1 C9 . 6_556 82.0(2) n
N1 Rh1 C9 . 6_556 93.74(13) n
N1 Rh1 C9 6_556 6_556 157.95(14) n
C10 Rh1 C9 6_556 . 82.0(2) n
C10 Rh1 C9 . . 37.2(2) n
N1 Rh1 C9 . . 157.95(14) n
N1 Rh1 C9 6_556 . 93.74(13) n
C9 Rh1 C9 6_556 . 90.5(2) n
N1 Rh1 X . . 91.1(2) y
X Rh1 X 6_556 . 87.6(2) y
C7 N1 C1 . . 115.3(2) n
C7 N1 Rh1 . . 120.6(2) n
C1 N1 Rh1 . . 123.6(2) n
C7 N2 C3 . . 122.7(3) n
C7 N2 C4 . . 113.1(2) n
C3 N2 C4 . . 122.3(3) n
C21 C1 N1 . . 114.1(4) n
C22 C1 N1 . . 118.9(7) n
C1 C21 C3 . . 115.1(6) n
C3 C22 C1 . . 119.2(13) n
C22 C3 N2 . . 111.5(7) n
N2 C3 C21 . . 109.3(4) n
N2 C4 C5 . . 103.6(3) n
C6 C5 C4 . . 105.8(3) n
C5 C6 C7 . . 104.2(3) n
N1 C7 N2 . . 126.8(3) n
N1 C7 C6 . . 124.8(3) n
N2 C7 C6 . . 108.4(3) n
C11 C8 C9 6_556 . 114.4(3) n
C10 C9 C8 . . 123.8(4) n
C10 C9 Rh1 . . 70.9(2) n
C8 C9 Rh1 . . 110.9(3) n
C9 C10 C11 . . 125.6(4) n
C9 C10 Rh1 . . 71.9(2) n
C11 C10 Rh1 . . 110.7(3) n
C8 C11 C10 6_556 . 114.6(4) n
F1 P1 F1 . 7_556 180.0 n
F1 P1 F3 . 7_556 90.5(2) n
F1 P1 F3 7_556 7_556 89.5(2) n
F1 P1 F3 . . 89.5(2) n
F1 P1 F3 7_556 . 90.5(2) n
F3 P1 F3 7_556 . 179.9960(10) n
F1 P1 F2 . 7_556 90.0(2) n
F1 P1 F2 7_556 7_556 90.0(2) n
F3 P1 F2 7_556 7_556 91.2(2) n
F3 P1 F2 . 7_556 88.8(2) n
F1 P1 F2 . . 90.0(2) n
F1 P1 F2 7_556 . 90.0(2) n
F3 P1 F2 7_556 . 88.8(2) n
F3 P1 F2 . . 91.2(2) n
F2 P1 F2 7_556 . 180.0 n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Rh1 C10 6_556 2.124(3) n
Rh1 C10 . 2.124(3) y
Rh1 N1 . 2.129(2) y
Rh1 N1 6_556 2.129(2) n
Rh1 C9 6_556 2.136(3) n
Rh1 C9 . 2.136(3) y
Rh1 X . 2.019(3) y
N1 C7 . 1.286(4) n
N1 C1 . 1.465(4) n
N2 C7 . 1.336(3) n
N2 C3 . 1.445(4) n
N2 C4 . 1.453(4) n
C1 C21 . 1.459(7) n
C1 C22 . 1.46(2) n
C21 C3 . 1.477(8) n
C22 C3 . 1.41(2) n
C4 C5 . 1.498(5) n
C5 C6 . 1.497(5) n
C6 C7 . 1.513(4) n
C8 C11 6_556 1.479(7) n
C8 C9 . 1.539(6) n
C9 C10 . 1.359(6) y
C10 C11 . 1.482(6) n
C11 C8 6_556 1.479(7) n
P1 F1 . 1.554(3) n
P1 F1 7_556 1.554(3) n
P1 F3 7_556 1.568(2) n
P1 F3 . 1.568(2) n
P1 F2 7_556 1.576(3) n
P1 F2 . 1.576(3) n
