#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/16/2201642.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_2201642
loop_
_publ_author_name
'Cabort, Amel'
'Therrien, Bruno'
'Bernauer, Klaus'
'Süss-Fink, Georg'
_publ_section_title
;
 [2,6-Bis(3,4-dihydro-2H-pyrrol-5-yl)pyridine]trichlororhodium(III)
 dibenzene solvate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m564
_journal_page_last               m565
_journal_paper_doi               10.1107/S1600536802016896
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Rh Cl3 (C13 H15 N3)], 2C6 H6'
_chemical_formula_moiety         'C25 H27 Cl3 N3 Rh, 2C6 H6'
_chemical_formula_sum            'C25 H27 Cl3 N3 Rh'
_chemical_formula_weight         578.76
_chemical_name_systematic
;
[RhCl₃{2,6-bis(3,4-dihydro-2H-pyrrol-5-yl)pyridine}] benzene solvate
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 100.12(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.434(2)
_cell_length_b                   10.630(2)
_cell_length_c                   20.948(4)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.87
_cell_measurement_theta_min      2.64
_cell_volume                     2506.5(8)
_computing_cell_refinement       'CELL in IPDS Software'
_computing_data_collection       'EXPOSE in IPDS Software (Stoe & Cie, 2000)'
_computing_data_reduction        'INTEGRATE in IPDS Software'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 0.81\%A
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'φ oscillation'
_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  0.049
_diffrn_reflns_av_sigmaI/netI    0.041
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8616
_diffrn_reflns_theta_full        25.9
_diffrn_reflns_theta_max         25.9
_diffrn_reflns_theta_min         2.6
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.019
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_correction_T_min  0.495
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.89
_refine_diff_density_min         -0.89
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.98
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2341
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.98
_refine_ls_R_factor_all          0.032
_refine_ls_R_factor_gt           0.026
_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)+(0.0361P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.058
_refine_ls_wR_factor_ref         0.059
_reflns_number_gt                1964
_reflns_number_total             2341
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            tk6079.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (4 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (4
times).

'_geom_angle_publ_flag' value 'Yes' changed to 'yes'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (8
times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2201642
_cod_database_fobs_code          2201642
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_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
C1 0.1801(2) 0.2301(2) 0.14892(11) 0.0233(5) Uani d . 1 . . C
H1A 0.1259 0.1887 0.1145 0.028 Uiso calc R 1 . . H
H1B 0.2262 0.1667 0.1756 0.028 Uiso calc R 1 . . H
C2 0.2621(2) 0.3215(2) 0.12068(12) 0.0261(5) Uani d . 1 . . C
H2A 0.2549 0.3096 0.0742 0.031 Uiso calc R 1 . . H
H2B 0.3443 0.3086 0.1408 0.031 Uiso calc R 1 . . H
C3 0.2202(2) 0.4544(2) 0.13595(11) 0.0217(5) Uani d . 1 . . C
H3A 0.2859 0.5055 0.1572 0.026 Uiso calc R 1 . . H
H3B 0.1814 0.4968 0.0969 0.026 Uiso calc R 1 . . H
C4 0.1353(2) 0.4272(2) 0.18001(11) 0.0175(5) Uani d . 1 . . C
C5 0.07004(19) 0.51704(19) 0.21466(10) 0.0172(5) Uani d . 1 . . C
C6 0.0721(2) 0.6479(2) 0.21414(12) 0.0227(5) Uani d . 1 . . C
H6 0.1206 0.6912 0.1903 0.027 Uiso calc R 1 . . H
C7 0.0000 0.7126(3) 0.2500 0.0239(7) Uani d S 1 . . C
H7 0.0000 0.8001 0.2500 0.029 Uiso calc SR 1 . . H
C8 0.4757(2) 0.1200(2) 0.01968(13) 0.0313(6) Uani d . 1 . . C
H8 0.4592 0.2006 0.0328 0.038 Uiso calc R 1 . . H
C9 0.4237(2) 0.0169(2) 0.04405(12) 0.0309(6) Uani d . 1 . . C
H9 0.3727 0.0281 0.0736 0.037 Uiso calc R 1 . . H
C10 0.4483(2) -0.1035(2) 0.02399(12) 0.0316(6) Uani d . 1 . . C
H10 0.4135 -0.1730 0.0401 0.038 Uiso calc R 1 . . H
C11 -0.0869(3) 0.0523(3) -0.04569(16) 0.0441(8) Uani d . 1 . . C
H11 -0.1459 0.0877 -0.0767 0.053 Uiso calc R 1 . . H
C12 -0.0982(3) 0.0525(3) 0.01880(16) 0.0423(7) Uani d . 1 . . C
H12 -0.1648 0.0884 0.0314 0.051 Uiso calc R 1 . . H
C13 -0.0119(3) 0.0002(3) 0.06396(13) 0.0429(8) Uani d . 1 . . C
H13 -0.0198 0.0000 0.1074 0.051 Uiso calc R 1 . . H
N1 0.11468(16) 0.30933(16) 0.18824(9) 0.0168(4) Uani d . 1 . . N
N2 0.0000 0.4572(2) 0.2500 0.0153(5) Uani d S 1 . . N
Cl1 -0.16151(5) 0.27971(5) 0.16405(2) 0.02139(14) Uani d . 1 . . Cl
Cl2 0.0000 0.05244(6) 0.2500 0.02382(19) Uani d S 1 . . Cl
Rh1 0.0000 0.27462(2) 0.2500 0.01405(9) Uani d S 1 . . Rh
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'
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
N1 C1 C2 . . 104.98(18) ?
N1 C1 H1A . . 110.8 ?
C2 C1 H1A . . 110.8 ?
N1 C1 H1B . . 110.8 ?
C2 C1 H1B . . 110.8 ?
H1A C1 H1B . . 108.8 ?
C1 C2 C3 . . 105.4(2) ?
C1 C2 H2A . . 110.7 ?
C3 C2 H2A . . 110.7 ?
C1 C2 H2B . . 110.7 ?
C3 C2 H2B . . 110.7 ?
H2A C2 H2B . . 108.8 ?
C4 C3 C2 . . 102.30(18) ?
C4 C3 H3A . . 111.3 ?
C2 C3 H3A . . 111.3 ?
C4 C3 H3B . . 111.3 ?
C2 C3 H3B . . 111.3 ?
H3A C3 H3B . . 109.2 ?
N1 C4 C3 . . 115.3(2) ?
N1 C4 C5 . . 116.2(2) ?
C3 C4 C5 . . 128.55(19) ?
N2 C5 C6 . . 119.4(2) ?
N2 C5 C4 . . 111.49(19) ?
C6 C5 C4 . . 129.1(2) ?
C7 C6 C5 . . 118.5(2) ?
C7 C6 H6 . . 120.7 ?
C5 C6 H6 . . 120.7 ?
C6 C7 C6 . 2 120.8(3) ?
C6 C7 H7 . . 119.6 ?
C6 C7 H7 2 . 119.6 ?
C10 C8 C9 5_655 . 120.3(2) ?
C10 C8 H8 5_655 . 119.8 ?
C9 C8 H8 . . 119.8 ?
C8 C9 C10 . . 119.6(3) ?
C8 C9 H9 . . 120.2 ?
C10 C9 H9 . . 120.2 ?
C8 C10 C9 5_655 . 120.1(2) ?
C8 C10 H10 5_655 . 120.0 ?
C9 C10 H10 . . 120.0 ?
C13 C11 C12 5 . 119.8(3) ?
C13 C11 H11 5 . 120.1 ?
C12 C11 H11 . . 120.1 ?
C13 C12 C11 . . 119.9(3) ?
C13 C12 H12 . . 120.0 ?
C11 C12 H12 . . 120.0 ?
C12 C13 C11 . 5 120.3(3) ?
C12 C13 H13 . . 119.9 ?
C11 C13 H13 5 . 119.9 ?
C4 N1 C1 . . 110.94(19) ?
C4 N1 Rh1 . . 114.49(15) ?
C1 N1 Rh1 . . 134.56(14) ?
C5 N2 C5 . 2 123.4(3) ?
C5 N2 Rh1 . . 118.29(13) ?
C5 N2 Rh1 2 . 118.29(13) ?
N2 Rh1 N1 . . 79.54(5) yes
N2 Rh1 N1 . 2 79.54(5) ?
N1 Rh1 N1 . 2 159.07(10) yes
N2 Rh1 Cl1 . 2 88.678(14) yes
N1 Rh1 Cl1 . 2 88.59(5) yes
N1 Rh1 Cl1 2 2 90.93(5) yes
N2 Rh1 Cl1 . . 88.678(14) ?
N1 Rh1 Cl1 . . 90.93(5) ?
N1 Rh1 Cl1 2 . 88.59(5) ?
Cl1 Rh1 Cl1 2 . 177.36(3) yes
N2 Rh1 Cl2 . . 180.0 ?
N1 Rh1 Cl2 . . 100.46(5) yes
N1 Rh1 Cl2 2 . 100.46(5) ?
Cl1 Rh1 Cl2 2 . 91.322(14) ?
Cl1 Rh1 Cl2 . . 91.322(14) yes
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
C1 N1 . 1.471(3) ?
C1 C2 . 1.539(3) ?
C1 H1A . 0.9700 ?
C1 H1B . 0.9700 ?
C2 C3 . 1.543(3) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C3 C4 . 1.480(3) ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
C4 N1 . 1.293(3) ?
C4 C5 . 1.478(3) ?
C5 N2 . 1.343(3) ?
C5 C6 . 1.392(3) ?
C6 C7 . 1.391(3) ?
C6 H6 . 0.9300 ?
C7 C6 2 1.391(3) ?
C7 H7 . 0.9300 ?
C8 C10 5_655 1.379(4) ?
C8 C9 . 1.386(4) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.391(4) ?
C9 H9 . 0.9300 ?
C10 C8 5_655 1.379(4) ?
C10 H10 . 0.9300 ?
C11 C13 5 1.373(5) ?
C11 C12 . 1.380(4) ?
C11 H11 . 0.9300 ?
C12 C13 . 1.360(5) ?
C12 H12 . 0.9300 ?
C13 C11 5 1.373(5) ?
C13 H13 . 0.9300 ?
N1 Rh1 . 2.031(2) yes
N2 C5 2 1.343(3) ?
N2 Rh1 . 1.941(2) yes
Cl1 Rh1 . 2.3424(9) yes
Cl2 Rh1 . 2.3618(8) yes
Rh1 N1 2 2.031(2) ?
Rh1 Cl1 2 2.3424(9) ?
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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
N1 C1 C2 C3 . . -10.5(2)
C1 C2 C3 C4 . . 9.3(2)
C2 C3 C4 N1 . . -5.1(2)
C2 C3 C4 C5 . . 176.1(2)
N1 C4 C5 N2 . . 0.7(2)
C3 C4 C5 N2 . . 179.50(19)
N1 C4 C5 C6 . . -178.6(2)
C3 C4 C5 C6 . . 0.2(4)
N2 C5 C6 C7 . . -0.7(3)
C4 C5 C6 C7 . . 178.54(18)
C5 C6 C7 C6 . 2 0.33(14)
C10 C8 C9 C10 5_655 . -0.2(4)
C8 C9 C10 C8 . 5_655 0.2(4)
C13 C11 C12 C13 5 . -0.3(4)
C11 C12 C13 C11 . 5 0.3(4)
C3 C4 N1 C1 . . -1.8(3)
C5 C4 N1 C1 . . 177.22(18)
C3 C4 N1 Rh1 . . 179.09(15)
C5 C4 N1 Rh1 . . -1.9(2)
C2 C1 N1 C4 . . 7.9(2)
C2 C1 N1 Rh1 . . -173.20(15)
C6 C5 N2 C5 . 2 0.34(14)
C4 C5 N2 C5 . 2 -179.00(19)
C6 C5 N2 Rh1 . . -179.66(14)
C4 C5 N2 Rh1 . . 1.00(19)
C5 N2 Rh1 N1 . . -1.56(11)
C5 N2 Rh1 N1 2 . 178.44(11)
C5 N2 Rh1 N1 . 2 178.44(11)
C5 N2 Rh1 N1 2 2 -1.56(11)
C5 N2 Rh1 Cl1 . 2 87.25(10)
C5 N2 Rh1 Cl1 2 2 -92.75(10)
C5 N2 Rh1 Cl1 . . -92.75(10)
C5 N2 Rh1 Cl1 2 . 87.25(10)
C5 N2 Rh1 Cl2 . . -14E1(5)
C5 N2 Rh1 Cl2 2 . 4E1(5)
C4 N1 Rh1 N2 . . 1.90(14)
C1 N1 Rh1 N2 . . -177.0(2)
C4 N1 Rh1 N1 . 2 1.90(13)
C1 N1 Rh1 N1 . 2 -177.0(2)
C4 N1 Rh1 Cl1 . 2 -87.01(14)
C1 N1 Rh1 Cl1 . 2 94.1(2)
C4 N1 Rh1 Cl1 . . 90.39(14)
C1 N1 Rh1 Cl1 . . -88.5(2)
C4 N1 Rh1 Cl2 . . -178.10(14)
C1 N1 Rh1 Cl2 . . 3.0(2)
