#------------------------------------------------------------------------------
#$Date: 2016-02-19 23:18:51 +0100 (Fri 19 de Feb de 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/93/2019307.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_2019307
loop_
_publ_author_name
'Vasiliev, Alexander D.'
'Molokeev, Maxim S.'
'Baidina, Iraida A.'
'Belyaev, Anatoly V.'
'Vorob'eva, Sofiya N.'
_publ_section_title
;
 Arrangement of Rh^3+^ ions in <i>fac</i>-triamminetrichloridorhodium from
 powder data and in <i>fac</i>-triamminetrinitratorhodium crystals twinned
 by merohedry
;
_journal_coeditor_code           LG3133
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1462
_journal_page_last               1466
_journal_paper_doi               10.1107/S010827011303076X
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Rh Cl3 (N H3)3]'
_chemical_formula_moiety         'Cl3 H9 N3 Rh'
_chemical_formula_sum            'Cl3 H9 N3 Rh'
_chemical_formula_weight         260.36
_chemical_name_systematic
;
<i>fac</i>-Triamminetrichloridorhodium(III)
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_cell_angle_alpha                90
_cell_angle_beta                 95.149(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.7279(3)
_cell_length_b                   9.7888(4)
_cell_length_c                   5.4611(2)
_cell_measurement_temperature    300
_cell_volume                     358.21(3)
_computing_cell_refinement       'TOPAS Rietveld (Bruker, 2008<i>b</i>)'
_computing_data_collection       'XRD Wizard (Bruker, 2007)'
_computing_data_reduction        'XRD Wizard (Bruker, 2007)'
_computing_structure_refinement  'TOPAS Rietveld (Bruker, 2008<i>b</i>)'
_computing_structure_solution
'TOPAS Phase annealing (Bruker, 2008<i>b</i>)'
_diffrn_ambient_temperature      300
_diffrn_measurement_device_type  'VANTEC linear detector'
_diffrn_measurement_method       \q--2\q
_diffrn_radiation_monochromator  none
_diffrn_radiation_type           'Cu K\a~1~'
_exptl_absorpt_coefficient_mu    28.779
_exptl_crystal_density_diffrn    2.414
_pd_char_colour                  yellow
_pd_meas_2theta_range_inc        0.016
_pd_meas_2theta_range_max        139.9869
_pd_meas_2theta_range_min        5
_pd_meas_scan_method             step
_pd_proc_ls_pref_orient_corr
;
PO-March Dollase - 1 Dir (0 0 1)
;
_pd_proc_ls_profile_function     PearsonVII
_pd_proc_ls_prof_R_factor        4.215
_pd_proc_ls_prof_wR_expected     1.538
_pd_proc_ls_prof_wR_factor       4.555
_pd_proc_number_of_points        8436.68125
_pd_spec_mount_mode              reflection
_refine_ls_goodness_of_fit_all   2.961
_refine_ls_goodness_of_fit_ref   2.961
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_number_parameters     78
_refine_ls_number_restraints     16
_refine_ls_shift/su_max          0.01000
_iucr_refine_instructions_details
;
do_errors
r_wp  4.514 r_exp  1.536 r_p  4.172 r_wp_dash  6.882 r_p_dash  5.271
r_exp_dash  2.341 weighted_Durbin_Watson  0.268 gof  2.940
xdd all.xye
x_calculation_step 0.016
   lam
      ymin_on_ymax 0.0001
      la 0.653817 lo 1.540596  lh 0.501844
      la 0.346183 lo 1.544493  lh 0.626579
 bkg  @  335.28  297.93 -60.74  139.16 -72.37  26.52 -5.15 16.89 -5.16
 One_on_X(@ , 13140.49952`_812.48034)
 Radius(217.5)
 Full_Axial_Model(12, @  7.140, @  11.361, @  5.05,  @  4.655)
 SD(@ , 0.03090`_0.00487)
 LP_Factor(90)
 str
 phase_name "Rh(NH3)3Cl3"
  space_group "P21/m"
PVII_Peak_Type(@ , 0.0001,@ , 0.0001,@ , 0.200,@ , 0.238,@ , 0.151,@ , 0.0001)
  a  @  6.72788`_0.00030
  b  @  9.78878`_0.00044
  c  @  5.46108`_0.00022
  be @   95.14886`_0.00175
  cell_volume  358.202899`_0.0269208452
  r_bragg  1.69496645
'# ANISO SIZE
 prm p2  0.09728`_0.02703 min 0.0001
 spherical_harmonics_hkl sh2
 sh_order  6 load sh_Cij_prm {
   y00   !sh2_c00  1.00000
   y20   sh2_c20   0.65452`_0.71965
   y22p  sh2_c22p -0.39420`_0.37459
   y22m  sh2_c22m -0.39197`_0.59945
   y40   sh2_c40   0.23518`_0.64248
   y42p  sh2_c42p -0.38450`_0.22984
   y42m  sh2_c42m  0.87521`_0.65496
   y44p  sh2_c44p -0.32906`_0.28423
   y44m  sh2_c44m  0.38309`_0.62035
   y60   sh2_c60   0.06164`_0.03324
   y62p  sh2_c62p -0.24400`_0.06187
   y62m  sh2_c62m  0.57632`_0.34590
   y64p  sh2_c64p  0.15991`_0.30937
   y64m  sh2_c64m  0.46529`_0.20104
   y66p  sh2_c66p  0.21632`_12594758.43957
   y66m  sh2_c66m  0.21632`_12594758.43965
   }
 gauss_fwhm = sh2 p2;
'# ATOMS
scale @  0.00522450072`_8.73e-005
site Rh    x @ 0.21960 y 0.25 z @ 0.48259  occ Rh   1
ADPs {@ 0.04927 @ 0.02206 @ 0.02313 0 @ 0.00033 0 }
site N1    x @  0.49572 y     0.25    z @  0.32728  occ N   1 beq bN2  3.1429
site N2    x @  0.11009 y  @  0.09654 z @  0.26036  occ N   1 beq bN1  2.5439
site Cl1   x @ -0.08076 y     0.25    z @  0.68286  occ Cl  1 beq @  3.0137
site Cl2   x @  0.35317 y  @  0.07745 z @  0.75253  occ Cl  1 beq @  2.7841
site H1   x  @  0.60581  y     0.25    z  @  0.45433 occ H 1.000 beq =1.5 bN2;
site H2   x  @  0.49760  y  @  0.17641 z  @  0.23192 occ H 1 beq beq =1.5 bN2;
site H3   x  @  0.14457  y  @  0.10745 z  @  0.10400 occ H 1.000 beq =1.5 bN1;
site H4   x  @  0.16459  y  @  0.00594 z  @  0.32479 occ H 1.000 beq =1.5 bN1;
site H5   x  @ -0.03449  y  @  0.10488 z  @  0.25379 occ H 1.000 beq =1.5 bN1;
    Distance_Restrain(H3 N2, 0.9, 0.92899`_0.03480, 0, 200000)
    Distance_Restrain(H4 N2, 0.9, 1.03076`_0.03916, 0, 200000)
    Distance_Restrain(H5 N2, 0.9, 0.97354`_0.03829, 0, 200000)
    Distance_Restrain(H2 N1, 0.9, 0.95510`_0.03149, 0, 200000)
    Distance_Restrain(H1 N1, 0.9, 0.90021`_0.04594, 0, 200000)
    Angle_Restrain(Rh N2 H3, 109, 112.06029`_1.93033, 0, 100)
    Angle_Restrain(Rh N2 H4, 109, 107.29689`_1.89780, 0, 100)
    Angle_Restrain(Rh N2 H5, 109, 105.51578`_1.81383, 0, 100)
    Angle_Restrain(H3 N2 H5, 109, 106.65733`_2.68587, 0, 100)
    Angle_Restrain(H3 N2 H4, 109, 111.28878`_2.61193, 0, 100)
    Angle_Restrain(H4 N2 H5, 109, 113.96237`_2.79036, 0, 100)
    Angle_Restrain(Rh N1 H2, 109, 107.79087`_1.90760, 0, 100)
    Angle_Restrain(Rh N1 H1, 109, 111.30892`_3.33695, 0, 100)
    Angle_Restrain(H2 N1 H1, 109, 108.55074`_2.41823, 0, 100)
view_structure
     PO(po, 0.89530`_0.00199, !angle2, 0 0 1)
Surface_Roughness_Suortti( , 0,  , 0.00010`_0.00293_LIMIT_MIN_0.0001)
;
_cod_data_source_file            lg3133.cif
_cod_data_source_block           I
_cod_original_cell_volume        358.21(2)
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               2019307
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
'-x, y+1/2, -z'
'x, -y+1/2, z'
loop_
_atom_site_type_symbol
_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_occupancy
Rh Rh 0.2195(2) 0.25 0.4826(2) 0.0318(7) Uani 1
N N1 0.4960(9) 0.25 0.3270(10) 0.040(4) Uiso 1
N N2 0.1122(6) 0.0942(3) 0.2608(7) 0.033(3) Uiso 1
Cl Cl1 -0.0810(5) 0.25 0.6825(6) 0.038(2) Uiso 1
Cl Cl2 0.3532(4) 0.0777(2) 0.7530(4) 0.0350(10) Uiso 1
H H1 0.606(8) 0.25 0.454(9) 0.06 Uiso 1
H H2 0.498(5) 0.176(3) 0.232(6) 0.06 Uiso 1
H H3 0.141(5) 0.110(3) 0.104(6) 0.05 Uiso 1
H H4 0.161(6) 0.006(4) 0.323(5) 0.05 Uiso 1
H H5 -0.035(6) 0.106(3) 0.253(6) 0.05 Uiso 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Rh 0.0490(15) 0.0229(12) 0.0229(11) 0 0.0003(6) 0
loop_
_diffrn_radiation_wavelength
1.5406
1.5444
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
N2 Rh1 N2 1_555 4_555 96.81(15) yes
N2 Rh1 N1 1_555 1_555 92.22(15) yes
N2 Rh1 Cl1 1_555 1_555 90.15(12) yes
N2 Rh1 Cl2 1_555 1_555 86.11(11) yes
N1 Rh1 Cl2 1_555 1_555 87.21(12) yes
Cl1 Rh1 Cl2 1_555 1_555 90.28(8) yes
Cl2 Rh1 Cl2 1_555 4_555 90.96(8) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Rh N1 2.113(5) yes
Rh1 N2 2.039(4) yes
Rh1 Cl1 2.382(4) yes
Rh1 Cl2 2.366(2) yes
N1 H1 0.96(5) ?
N1 H2 0.89(3) ?
N2 H3 0.91(3) ?
N2 H4 0.98(4) ?
N2 H5 0.99(4) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1 Cl1 1_655 0.97(5) 2.35(5) 3.297(7) 166(4) yes
N1 H2 Cl2 2_656 0.89(3) 2.68(3) 3.405(4) 140(3) yes
N2 H3 Cl2 1_554 0.91(3) 2.51(3) 3.340(5) 152(3) yes
N2 H4 Cl1 3_546 0.98(4) 2.56(4) 3.392(3) 143(3) yes
N2 H5 Cl2 2_556 0.99(4) 2.79(4) 3.550(5) 134(3) yes
