#------------------------------------------------------------------------------
#$Date: 2016-02-19 23:18:51 +0100 (Fri 19 de Feb de 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/93/2019308.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_2019308
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 Rh³⁺ ions in fac-triamminetrichloridorhodium from
 powder data and in fac-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 (N O3)3 (N H3)3]'
_chemical_formula_moiety         'H9 N6 O9 Rh'
_chemical_formula_sum            'H9 N6 O9 Rh'
_chemical_formula_weight         340.04
_chemical_name_systematic
;
fac-Triamminetrinitratorhodium(III)
;
_space_group_IT_number           143
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3'
_symmetry_space_group_name_H-M   'P 3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            1
_cell_length_a                   7.4960(10)
_cell_length_b                   7.4960(10)
_cell_length_c                   5.2560(8)
_cell_measurement_reflns_used    3627
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      32.93
_cell_measurement_theta_min      3.14
_cell_volume                     255.77(6)
_computing_cell_refinement       'APEX2 (Bruker, 2008a)'
_computing_data_collection       'APEX2 (Bruker, 2008a)'
_computing_data_reduction        'SAINT (Bruker, 2008a)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'phi and 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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3780
_diffrn_reflns_theta_full        33.02
_diffrn_reflns_theta_max         33.02
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    1.72
_exptl_absorpt_correction_T_max  0.7822
_exptl_absorpt_correction_T_min  0.5458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             168
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.320
_refine_ls_abs_structure_details 'Flack (1983), 230 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.03(9)
_refine_ls_extinction_coef       0.035(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         879
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0191
_refine_ls_R_factor_gt           0.0191
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0355P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0481
_refine_ls_wR_factor_ref         0.0481
_reflns_number_gt                879
_reflns_number_total             879
_reflns_threshold_expression     I>2sigma(I)
_iucr_refine_instructions_details
;
TITL Rh(NH3)3(NO3)3 in P3
CELL 0.71073   7.4960    7.4960    5.2560   90.000  90.000 120.000
ZERR    1.00   0.0010    0.0010    0.0008    0.000   0.000   0.000
LATT  -1
SYMM -y, x-y, z
SYMM y-x, -x, z
SFAC O Rh N H
UNIT 9 9 1 6
TEMP 23.000
SIZE 0.15 0.15 0.4
L.S. 8
acta
BOND $H
FMAP 2
PLAN 20
twin 0 1 0 1 0 0 0 0 -1
WGHT    0.035500
EXTI    0.035333
BASF   0.50374
FVAR       0.56747   0.80393
RH1   2    0.000000    0.000000   10.500000    20.33333    0.01485    0.01485 =
         0.01332    0.00000    0.00000    0.00742
RH2   2    0.000000    0.000000   -0.035176   -20.33333    0.02078    0.02078 =
         0.00676    0.00000    0.00000    0.01039
O1    1    0.202510    0.000627    0.243017    11.00000    0.02219    0.05004 =
         0.02541    0.00016    0.00486    0.02373
N1    3    0.224500    0.223940    0.741311    11.00000    0.02135    0.02722 =
         0.02929    0.00059    0.00048    0.00058
N2    3    0.373189    0.000644    0.277290    11.00000    0.04055    0.10098 =
         0.04984    0.00020    0.00279    0.04973
O2    1    0.424798   -0.001336    0.496882    11.00000    0.08062    0.21201 =
         0.05522    0.00003   -0.02340    0.10629
O3    1    0.470787    0.000083    0.086682    11.00000    0.11012    0.21517 =
         0.08242    0.00008    0.04849    0.10521
HKLF 4
END
;
_cod_data_source_file            lg3133.cif
_cod_data_source_block           II
_cod_original_cell_volume        255.77(7)
_cod_database_code               2019308
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, 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_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Rh Rh1 0.0000 0.0000 0.5000 0.01434(9) Uani d SP 0.8039(18) 3
Rh Rh2 0.0000 0.0000 -0.0352(3) 0.0161(7) Uani d SP 0.1961(18) 3
O O1 0.2025(13) 0.001(2) 0.2430(16) 0.0300(10) Uani d . 1 1
N N1 0.2245(15) 0.2239(16) 0.741(2) 0.0311(12) Uani d . 1 1
N N2 0.3732(7) 0.0006(9) 0.2773(9) 0.0574(15) Uani d . 1 1
O O2 0.4248(16) -0.001(3) 0.4969(19) 0.101(2) Uani d . 1 1
O O3 0.4708(14) 0.0001(19) 0.0867(13) 0.125(3) Uani d . 1 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
Rh1 0.01485(9) 0.01485(9) 0.01332(17) 0.00742(5) 0.000 0.000
Rh2 0.0208(5) 0.0208(5) 0.0068(16) 0.0104(2) 0.000 0.000
O1 0.0222(19) 0.050(2) 0.0254(15) 0.0237(18) 0.0049(17) 0.0002(14)
N1 0.021(2) 0.027(3) 0.0293(18) 0.0006(17) 0.0005(18) 0.001(2)
N2 0.041(2) 0.101(4) 0.050(3) 0.050(3) 0.0028(19) 0.000(3)
O2 0.081(6) 0.212(7) 0.055(3) 0.106(6) -0.023(3) 0.000(3)
O3 0.110(7) 0.215(9) 0.082(5) 0.105(7) 0.048(5) 0.000(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
N N 0.0061 0.0033 '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'
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 Rh1 N1 . 2 87.5(4) yes
N1 Rh1 N1 . 3 87.5(4) ?
N1 Rh1 N1 2 3 87.5(4) ?
N1 Rh1 O1 . 3 175.3(5) yes
N1 Rh1 O1 2 3 96.0(6) yes
N1 Rh1 O1 3 3 95.8(6) yes
N1 Rh1 O1 . . 95.8(6) ?
N1 Rh1 O1 2 . 175.3(4) ?
N1 Rh1 O1 3 . 96.0(6) ?
O1 Rh1 O1 3 . 80.6(3) yes
N1 Rh1 O1 . 2 96.0(6) ?
N1 Rh1 O1 2 2 95.8(6) ?
N1 Rh1 O1 3 2 175.3(4) ?
O1 Rh1 O1 3 2 80.6(3) ?
O1 Rh1 O1 . 2 80.6(3) ?
N1 Rh1 Rh2 . 1_556 53.0(3) ?
N1 Rh1 Rh2 2 1_556 53.0(3) ?
N1 Rh1 Rh2 3 1_556 53.0(3) ?
O1 Rh1 Rh2 3 1_556 131.7(2) ?
O1 Rh1 Rh2 . 1_556 131.7(2) ?
O1 Rh1 Rh2 2 1_556 131.7(2) ?
N1 Rh1 Rh2 . . 127.0(3) ?
N1 Rh1 Rh2 2 . 127.0(3) ?
N1 Rh1 Rh2 3 . 127.0(3) ?
O1 Rh1 Rh2 3 . 48.3(2) ?
O1 Rh1 Rh2 . . 48.3(2) ?
O1 Rh1 Rh2 2 . 48.3(2) ?
Rh2 Rh1 Rh2 1_556 . 180.0000(10) ?
O1 Rh2 O1 2 . 77.1(3) yes
O1 Rh2 O1 2 3 77.1(3) ?
O1 Rh2 O1 . 3 77.1(3) ?
O1 Rh2 N1 2 2_554 95.8(5) yes
O1 Rh2 N1 . 2_554 171.0(5) yes
O1 Rh2 N1 3 2_554 96.0(6) yes
O1 Rh2 N1 2 3_554 171.0(5) ?
O1 Rh2 N1 . 3_554 96.0(6) ?
O1 Rh2 N1 3 3_554 95.8(5) ?
N1 Rh2 N1 2_554 3_554 90.4(4) yes
O1 Rh2 N1 2 1_554 96.0(6) ?
O1 Rh2 N1 . 1_554 95.8(5) ?
O1 Rh2 N1 3 1_554 171.0(5) ?
N1 Rh2 N1 2_554 1_554 90.4(4) ?
N1 Rh2 N1 3_554 1_554 90.4(4) ?
O1 Rh2 Rh1 2 1_554 134.0(2) ?
O1 Rh2 Rh1 . 1_554 134.0(2) ?
O1 Rh2 Rh1 3 1_554 134.0(2) ?
N1 Rh2 Rh1 2_554 1_554 55.0(3) ?
N1 Rh2 Rh1 3_554 1_554 55.0(3) ?
N1 Rh2 Rh1 1_554 1_554 55.0(3) ?
O1 Rh2 Rh1 2 . 46.0(2) ?
O1 Rh2 Rh1 . . 46.0(2) ?
O1 Rh2 Rh1 3 . 46.0(2) ?
N1 Rh2 Rh1 2_554 . 125.0(3) ?
N1 Rh2 Rh1 3_554 . 125.0(3) ?
N1 Rh2 Rh1 1_554 . 125.0(3) ?
Rh1 Rh2 Rh1 1_554 . 180.0 ?
N2 O1 Rh1 . . 130.3(6) ?
N2 O1 Rh2 . . 144.0(6) ?
Rh1 O1 Rh2 . . 85.7(2) ?
Rh1 N1 Rh2 . 1_556 72.0(2) ?
O3 N2 O2 . . 124.9(6) ?
O3 N2 O1 . . 118.2(6) ?
O2 N2 O1 . . 116.9(6) ?
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 N1 . 2.106(9) yes
Rh1 N1 2 2.106(9) ?
Rh1 N1 3 2.106(9) ?
Rh1 O1 3 2.030(8) yes
Rh1 O1 . 2.030(7) ?
Rh1 O1 2 2.030(7) ?
Rh1 Rh2 1_556 2.4431(18) ?
Rh1 Rh2 . 2.8129(18) ?
Rh2 O1 2 2.106(7) ?
Rh2 O1 . 2.106(7) ?
Rh2 O1 3 2.106(7) ?
Rh2 N1 2_554 2.051(9) ?
Rh2 N1 3_554 2.051(9) ?
Rh2 N1 1_554 2.051(9) ?
Rh2 Rh1 1_554 2.4431(18) ?
O1 N2 . 1.292(8) yes
N1 Rh2 1_556 2.051(9) ?
N2 O3 . 1.242(7) yes
N2 O2 . 1.220(10) yes
