#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/14/2201420.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_2201420
loop_
_publ_author_name
'Harris, Pernille'
'Kofod, Pauli'
_publ_section_title
;
 A methyl-coordinated RhIII ion in
 methylpentaamminerhodium(III)--chloropentaamminerhodium(III)--dithionate
 (0.73/2.27/3)
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m460
_journal_page_last               m462
_journal_paper_doi               10.1107/S1600536802013466
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac
'[Rh (C H3) (N H3)5 ]0.73 [Rh Cl (N H3)5]2.27 (S2 O6)3'
_chemical_formula_moiety         '0.73Rh N5 C H18, 2.27Rh N5 Cl H15, 3S2 O6'
_chemical_formula_sum            'C0.73 H47.19 Cl2.27 N15 O18 Rh3 S6'
_chemical_formula_weight         1135.58
_chemical_name_systematic        ?
_space_group_IT_number           8
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'I -2y'
_symmetry_space_group_name_H-M   'I 1 m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 97.290(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.271(2)
_cell_length_b                   27.205(3)
_cell_length_c                   9.871(2)
_cell_measurement_reflns_used    474
_cell_measurement_temperature    122.0(10)
_cell_measurement_theta_max      31.0
_cell_measurement_theta_min      4.4
_cell_volume                     1670.4(7)
_computing_cell_refinement       'DIRAX (Duisenberg, 1992)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction
;
EvalCCD (Duisenberg, 1998) and DREAD (Blessing, 1987)
;
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      122.0(10)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'θ and φ'
_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  0.0568
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34422
_diffrn_reflns_theta_full        35.02
_diffrn_reflns_theta_max         35.02
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.109
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Gaussian integration (Coppens, 1970)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.299
_refine_diff_density_min         -1.680
_refine_ls_abs_structure_details 'Flack (1983), 0000 Friedel pairs'
_refine_ls_abs_structure_Flack   0.43(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         7322
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0598P)²+6.9449P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1020
_reflns_number_gt                7148
_reflns_number_total             7322
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cm6013.cif
_cod_data_source_block           I
_cod_original_cell_volume        1670.4
_cod_original_sg_symbol_H-M      'I m'
_cod_database_code               2201420
_cod_database_fobs_code          2201420
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z'
'x+1/2, y+1/2, z+1/2'
'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
Rh2 0.96197(3) 0.166778(9) 0.62172(2) 0.01111(5) Uani d D 1 . . Rh
N21 0.8546(6) 0.11675(12) 0.7539(3) 0.0144(6) Uani d . 1 . . N
H21A 0.9600 0.0959 0.7826 0.022 Uiso calc R 1 . . H
H21B 0.7435 0.1002 0.7111 0.022 Uiso calc R 1 . . H
H21C 0.8137 0.1325 0.8253 0.022 Uiso calc R 1 . . H
N22 1.2650(7) 0.15910(15) 0.7268(4) 0.0214(7) Uani d . 1 . . N
H22A 1.2813 0.1801 0.7966 0.032 Uiso calc R 1 . . H
H22B 1.3627 0.1654 0.6712 0.032 Uiso calc R 1 . . H
H22C 1.2821 0.1285 0.7582 0.032 Uiso calc R 1 . . H
N23 0.8991(6) 0.22508(13) 0.7440(3) 0.0167(6) Uani d . 1 . . N
H23A 0.8660 0.2138 0.8233 0.025 Uiso calc R 1 . . H
H23B 0.7893 0.2424 0.7026 0.025 Uiso calc R 1 . . H
H23C 1.0149 0.2442 0.7588 0.025 Uiso calc R 1 . . H
N24 1.0663(6) 0.21550(15) 0.4822(4) 0.0188(6) Uani d . 1 . . N
H24A 1.1241 0.2418 0.5261 0.028 Uiso calc R 1 . . H
H24B 0.9552 0.2247 0.4224 0.028 Uiso calc R 1 . . H
H24C 1.1643 0.2009 0.4382 0.028 Uiso calc R 1 . . H
N25 1.0187(7) 0.10934(15) 0.4902(4) 0.0203(7) Uani d . 1 . . N
H25A 1.1585 0.1078 0.4828 0.030 Uiso calc R 1 . . H
H25B 0.9455 0.1147 0.4083 0.030 Uiso calc R 1 . . H
H25C 0.9762 0.0811 0.5235 0.030 Uiso calc R 1 . . H
Cl 0.61140(19) 0.17248(4) 0.50636(11) 0.02194(19) Uani d D 1 . . Cl
Rh1 0.48747(5) 0.0000 0.15369(3) 0.01348(8) Uani d SD 1 . . Rh
N13 0.5745(7) 0.05419(14) 0.0245(4) 0.0195(7) Uani d . 1 . . N
H13A 0.6521 0.0410 -0.0357 0.029 Uiso calc R 1 . . H
H13B 0.6522 0.0770 0.0731 0.029 Uiso calc R 1 . . H
H13C 0.4568 0.0679 -0.0196 0.029 Uiso calc R 1 . . H
N12 0.4006(8) 0.05356(17) 0.2846(4) 0.0249(8) Uani d . 1 . . N
H12A 0.3951 0.0826 0.2427 0.037 Uiso calc R 1 . . H
H12B 0.4972 0.0547 0.3588 0.037 Uiso calc R 1 . . H
H12C 0.2720 0.0465 0.3086 0.037 Uiso calc R 1 . . H
Cl1 0.8391(8) 0.0000 0.2738(5) 0.0126(12) Uiso d SPD 0.270(10) . . Cl
C11 0.782(3) 0.0000 0.2567(17) 0.041(3) Uiso d SP 0.73(2) . . C
N11 0.1657(10) 0.0000 0.0412(6) 0.0221(10) Uani d S 1 . . N
H11A 0.1179 0.0308 0.0312 0.033 Uiso calc PR 0.50 . . H
H11B 0.0780 -0.0173 0.0869 0.033 Uiso calc PR 0.50 . . H
H11C 0.1695 -0.0134 -0.0407 0.033 Uiso calc PR 0.50 . . H
S3 0.5967(3) 0.0000 0.64904(13) 0.0166(2) Uani d S 1 . . S
S4 0.2697(3) 0.0000 0.68079(18) 0.0222(3) Uani d S 1 . . S
O32 0.6211(6) -0.04480(10) 0.5726(3) 0.0252(7) Uani d . 1 . . O
O31 0.7225(8) 0.0000 0.7845(4) 0.0180(8) Uani d S 1 . . O
O42 0.2457(6) 0.04457(11) 0.7579(4) 0.0270(7) Uani d . 1 . . O
O41 0.1538(10) 0.0000 0.5435(6) 0.0352(14) Uani d S 1 . . O
S1 0.82960(19) 0.17203(3) 0.12449(10) 0.01545(17) Uani d . 1 . . S
S2 1.15676(19) 0.16083(3) 0.09385(12) 0.01922(19) Uani d . 1 . . S
O11 0.7843(6) 0.13023(11) 0.2063(3) 0.0240(6) Uani d . 1 . . O
O12 0.8273(5) 0.21944(10) 0.1934(3) 0.0216(5) Uani d . 1 . . O
O13 0.7098(6) 0.17221(11) -0.0127(3) 0.0173(6) Uani d . 1 . . O
O21 1.2712(8) 0.16123(12) 0.2308(4) 0.0313(9) Uani d . 1 . . O
O22 1.2068(5) 0.20179(11) 0.0079(4) 0.0266(6) Uani d . 1 . . O
O23 1.1573(5) 0.11329(11) 0.0254(4) 0.0251(6) Uani d . 1 . . O
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Rh Rh -1.1178 0.9187 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
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
N22 Rh2 N21 . . 88.21(15) yes
N22 Rh2 N23 . . 90.91(15) yes
N21 Rh2 N23 . . 92.04(14) yes
N22 Rh2 N24 . . 92.90(16) yes
N21 Rh2 N24 . . 177.83(15) yes
N23 Rh2 N24 . . 89.81(15) yes
N22 Rh2 N25 . . 91.04(15) yes
N21 Rh2 N25 . . 89.69(14) yes
N23 Rh2 N25 . . 177.43(15) yes
N24 Rh2 N25 . . 88.42(16) yes
N22 Rh2 Cl . . 177.54(13) yes
N21 Rh2 Cl . . 89.40(10) yes
N23 Rh2 Cl . . 89.79(11) yes
N24 Rh2 Cl . . 89.46(11) yes
N25 Rh2 Cl . . 88.33(11) yes
Rh2 N21 H21A . . 109.5 no
Rh2 N21 H21B . . 109.5 no
H21A N21 H21B . . 109.5 no
Rh2 N21 H21C . . 109.5 no
H21A N21 H21C . . 109.5 no
H21B N21 H21C . . 109.5 no
Rh2 N22 H22A . . 109.5 no
Rh2 N22 H22B . . 109.5 no
H22A N22 H22B . . 109.5 no
Rh2 N22 H22C . . 109.5 no
H22A N22 H22C . . 109.5 no
H22B N22 H22C . . 109.5 no
Rh2 N23 H23A . . 109.5 no
Rh2 N23 H23B . . 109.5 no
H23A N23 H23B . . 109.5 no
Rh2 N23 H23C . . 109.5 no
H23A N23 H23C . . 109.5 no
H23B N23 H23C . . 109.5 no
Rh2 N24 H24A . . 109.5 no
Rh2 N24 H24B . . 109.5 no
H24A N24 H24B . . 109.5 no
Rh2 N24 H24C . . 109.5 no
H24A N24 H24C . . 109.5 no
H24B N24 H24C . . 109.5 no
Rh2 N25 H25A . . 109.5 no
Rh2 N25 H25B . . 109.5 no
H25A N25 H25B . . 109.5 no
Rh2 N25 H25C . . 109.5 no
H25A N25 H25C . . 109.5 no
H25B N25 H25C . . 109.5 no
C11 Rh1 N12 . . 89.0(3) yes
N12 Rh1 N12 . 2 89.7(3) yes
C11 Rh1 N13 . 2 90.8(3) yes
N12 Rh1 N13 . 2 179.34(18) yes
N12 Rh1 N13 . . 89.67(16) yes
N13 Rh1 N13 2 . 91.0(2) yes
C11 Rh1 N11 . . 180.0(5) yes
N12 Rh1 N11 . . 91.04(17) yes
N13 Rh1 N11 . . 89.17(15) yes
N12 Rh1 Cl1 . . 89.40(15) yes
N13 Rh1 Cl1 . . 90.40(14) yes
N11 Rh1 Cl1 . . 179.4(2) yes
Rh1 N13 H13A . . 109.5 no
Rh1 N13 H13B . . 109.5 no
H13A N13 H13B . . 109.5 no
Rh1 N13 H13C . . 109.5 no
H13A N13 H13C . . 109.5 no
H13B N13 H13C . . 109.5 no
Rh1 N12 H12A . . 109.5 no
Rh1 N12 H12B . . 109.5 no
H12A N12 H12B . . 109.5 no
Rh1 N12 H12C . . 109.5 no
H12A N12 H12C . . 109.5 no
H12B N12 H12C . . 109.5 no
Rh1 N11 H11A . . 109.5 no
Rh1 N11 H11B . . 109.5 no
H11A N11 H11B . . 109.5 no
Rh1 N11 H11C . . 109.5 no
H11A N11 H11C . . 109.5 no
H11B N11 H11C . . 109.5 no
O32 S3 O32 . 2 114.2(3) no
O32 S3 O31 . . 113.23(16) no
O32 S3 S4 . . 104.19(18) no
O31 S3 S4 . . 106.6(2) no
O42 S4 O42 . 2 113.5(3) no
O42 S4 O41 . . 114.60(19) no
O42 S4 S3 . . 104.20(15) no
O41 S4 S3 . . 104.0(3) no
O11 S1 O12 . . 114.93(18) no
O11 S1 O13 . . 113.95(19) no
O12 S1 O13 . . 113.22(17) no
O11 S1 S2 . . 103.18(16) no
O12 S1 S2 . . 105.00(15) no
O13 S1 S2 . . 105.03(16) no
O21 S2 O22 . . 114.8(2) no
O21 S2 O23 . . 114.1(2) no
O22 S2 O23 . . 113.2(2) no
O21 S2 S1 . . 103.8(2) no
O22 S2 S1 . . 104.77(14) no
O23 S2 S1 . . 104.55(15) no
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
Rh2 N22 . 2.057(4) yes
Rh2 N21 . 2.057(4) yes
Rh2 N23 . 2.061(4) yes
Rh2 N24 . 2.076(4) yes
Rh2 N25 . 2.091(4) yes
Rh2 Cl . 2.3492(12) yes
N21 H21A . 0.8900 no
N21 H21B . 0.8900 no
N21 H21C . 0.8900 no
N22 H22A . 0.8900 no
N22 H22B . 0.8900 no
N22 H22C . 0.8900 no
N23 H23A . 0.8900 no
N23 H23B . 0.8900 no
N23 H23C . 0.8900 no
N24 H24A . 0.8900 no
N24 H24B . 0.8900 no
N24 H24C . 0.8900 no
N25 H25A . 0.8900 no
N25 H25B . 0.8900 no
N25 H25C . 0.8900 no
Rh1 C11 . 1.99(2) yes
Rh1 N12 . 2.066(4) yes
Rh1 N13 . 2.068(4) yes
Rh1 N11 . 2.177(6) yes
Rh1 Cl1 . 2.368(5) yes
N13 H13A . 0.8900 no
N13 H13B . 0.8900 no
N13 H13C . 0.8900 no
N12 H12A . 0.8900 no
N12 H12B . 0.8900 no
N12 H12C . 0.8900 no
N11 H11A . 0.8900 no
N11 H11B . 0.8900 no
N11 H11C . 0.8900 no
S3 O32 . 1.451(3) no
S3 O31 . 1.463(5) no
S3 S4 . 2.113(3) no
S4 O42 . 1.450(3) no
S4 O41 . 1.454(5) no
S1 O11 . 1.444(3) no
S1 O12 . 1.459(3) no
S1 O13 . 1.463(3) no
S1 S2 . 2.133(2) no
S2 O21 . 1.448(4) no
S2 O22 . 1.458(4) no
S2 O23 . 1.460(3) no
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
_geom_torsion_publ_flag
O32 S3 S4 O42 . . 179.6(2) no
O31 S3 S4 O42 . . 59.64(17) no
O32 S3 S4 O42 . 2 60.3(2) no
O32 S3 S4 O41 2 . 60.01(14) no
O31 S3 S4 O41 . . 180.0 no
O11 S1 S2 O21 . . -60.8(2) no
O12 S1 S2 O21 . . 59.9(2) no
O13 S1 S2 O21 . . 179.5(2) no
O11 S1 S2 O22 . . 178.43(19) no
O12 S1 S2 O22 . . -60.8(2) no
O13 S1 S2 O22 . . 58.8(2) no
O11 S1 S2 O23 . . 59.1(2) no
O12 S1 S2 O23 . . 179.8(2) no
O13 S1 S2 O23 . . -60.5(2) no
