#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:40:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179198 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/36/4313662.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4313662
loop_
_publ_author_name
'Piotr Smoleński'
'Florian P. Pruchnik'
'Zbigniew Ciunik'
'Tadeusz Lis'
_publ_contact_author
;
Florian P. Pruchnik
Faculty of Chemistry, University of Wroclaw,
14. F. Joliot-Curie Street, 50-383 Wroclaw,
Poland
;
_publ_contact_author_email       pruchnik@wchuwr.chem.uni.wroc.pl
_publ_section_title
;
 New Rhodium(III) and Ruthenium(II) Water-Soluble Complexes with
 3,5-Diaza-1-methyl-1-azonia-7-phosphatricyclo[3.3.1.13,7]decane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3318
_journal_page_last               3322
_journal_paper_doi               10.1021/ic034044v
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         '[RhI4{P(CH2)6N2NCH3}2]I'
_chemical_formula_sum            'C14 H30 I5 N6 P2 Rh'
_chemical_formula_weight         1081.79
_chemical_name_common
'bis{diazamethylazoniaphosphaadamantane} tetraiodorhodium(III) iodide'
_chemical_name_systematic
; 
    (OC-6-11)-{bis(3,5-diaza-1-methyl-1-azonia-7
    -phosphatricyclo[3.3.1.1^3,7]decane}tetraiodo
    -rhodium(III) iodide
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                90.00
_cell_angle_beta                 96.27(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.803(3)
_cell_length_b                   9.295(3)
_cell_length_c                   13.786(3)
_cell_measurement_temperature    100(2)
_cell_volume                     1376.0(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.839
_diffrn_measured_fraction_theta_max 0.839
_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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7535
_diffrn_reflns_theta_full        28.73
_diffrn_reflns_theta_max         28.73
_diffrn_reflns_theta_min         3.69
_exptl_absorpt_coefficient_mu    6.360
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.244
_exptl_crystal_density_diffrn    2.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.232
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         3182
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0270P)²+8.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0728
_reflns_number_gt                2898
_reflns_number_total             3182
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034044vsi20030326_081136_1.cif
_cod_data_source_block           rhic
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+8.5000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+8.5000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4313662
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_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
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh Rh 0.5000 0.5000 0.5000 0.01252(10) Uani 1 d S . .
I1 I 0.65458(3) 0.53696(3) 0.66572(2) 0.01615(8) Uani 1 d . . .
I2 I 0.52168(3) 0.77900(3) 0.45469(2) 0.01740(9) Uani 1 d . . .
I3 I 0.92627(15) 0.57142(8) 0.9179(2) 0.0164(4) Uani 0.460(5) d P . .
I31 I 0.9120(8) 0.5698(12) 0.869(3) 0.027(6) Uani 0.040(5) d P . .
P P 0.33151(11) 0.54290(12) 0.58661(8) 0.0148(2) Uani 1 d . . .
N1 N 0.2278(4) 0.5026(4) 0.7616(3) 0.0165(7) Uani 1 d . . .
N2 N 0.0849(4) 0.4929(5) 0.6100(3) 0.0204(8) Uani 1 d . . .
N3 N 0.1710(4) 0.7224(4) 0.6695(3) 0.0212(8) Uani 1 d . . .
C1 C 0.3446(4) 0.4761(5) 0.7130(3) 0.0155(8) Uani 1 d . . .
H11 H 0.3620 0.3715 0.7130 0.019 Uiso 1 calc R . .
H12 H 0.4157 0.5242 0.7512 0.019 Uiso 1 calc R . .
C2 C 0.1796(4) 0.4630(6) 0.5428(4) 0.0216(9) Uani 1 d . . .
H21 H 0.1508 0.5023 0.4775 0.026 Uiso 1 calc R . .
H22 H 0.1892 0.3576 0.5363 0.026 Uiso 1 calc R . .
C3 C 0.2782(4) 0.7273(5) 0.6119(4) 0.0208(9) Uani 1 d . . .
H31 H 0.3472 0.7816 0.6483 0.025 Uiso 1 calc R . .
H32 H 0.2541 0.7780 0.5495 0.025 Uiso 1 calc R . .
C4 C 0.2459(3) 0.4443(4) 0.8631(3) 0.0231(10) Uani 1 d . . .
H41 H 0.1707 0.4617 0.8952 0.028 Uiso 1 calc R . .
H42 H 0.3170 0.4924 0.8998 0.028 Uiso 1 calc R . .
H43 H 0.2619 0.3406 0.8609 0.028 Uiso 1 calc R . .
C5 C 0.1145(3) 0.4297(4) 0.7042(3) 0.0204(9) Uani 1 d R . .
H51 H 0.1325 0.3261 0.6965 0.025 Uiso 1 calc R . .
H52 H 0.0417 0.4380 0.7416 0.025 Uiso 1 calc R . .
C6 C 0.2014(4) 0.6638(5) 0.7652(3) 0.0195(9) Uani 1 d . . .
H61 H 0.1313 0.6807 0.8044 0.023 Uiso 1 calc R . .
H62 H 0.2755 0.7138 0.7977 0.023 Uiso 1 calc R . .
C7 C 0.0630(5) 0.6472(6) 0.6197(4) 0.0248(10) Uani 1 d . . .
H71 H -0.0095 0.6619 0.6567 0.030 Uiso 1 calc R . .
H72 H 0.0425 0.6894 0.5540 0.030 Uiso 1 calc R . .
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'
P P 0.1023 0.0942 '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'
I I -0.4742 1.8119 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P Rh P 180.0 . 3_666 ?
P Rh I2 87.30(3) . 3_666 ?
P Rh I2 92.70(3) 3_666 3_666 ?
P Rh I2 92.70(3) . . ?
P Rh I2 87.30(3) 3_666 . ?
I2 Rh I2 180.0 3_666 . ?
P Rh I1 89.44(4) . . ?
P Rh I1 90.56(4) 3_666 . ?
I2 Rh I1 89.292(11) 3_666 . ?
I2 Rh I1 90.708(11) . . ?
P Rh I1 90.56(4) . 3_666 ?
P Rh I1 89.44(4) 3_666 3_666 ?
I2 Rh I1 90.708(11) 3_666 3_666 ?
I2 Rh I1 89.292(11) . 3_666 ?
I1 Rh I1 180.0 . 3_666 ?
I31 I3 I3 143.6(12) . 3_767 ?
C1 P C2 98.5(2) . . ?
C1 P C3 97.3(2) . . ?
C2 P C3 98.7(2) . . ?
C1 P Rh 116.49(14) . . ?
C2 P Rh 118.92(16) . . ?
C3 P Rh 122.24(16) . . ?
C4 N1 C1 109.0(3) . . ?
C4 N1 C6 109.3(3) . . ?
C1 N1 C6 110.0(3) . . ?
C4 N1 C5 109.7(3) . . ?
C1 N1 C5 110.8(3) . . ?
C6 N1 C5 108.0(3) . . ?
C5 N2 C7 110.0(3) . . ?
C5 N2 C2 112.9(4) . . ?
C7 N2 C2 111.8(4) . . ?
C6 N3 C7 109.9(4) . . ?
C6 N3 C3 113.2(4) . . ?
C7 N3 C3 113.2(4) . . ?
N1 C1 P 112.5(3) . . ?
N1 C1 H11 109.1 . . ?
P C1 H11 109.1 . . ?
N1 C1 H12 109.1 . . ?
P C1 H12 109.1 . . ?
H11 C1 H12 107.8 . . ?
N2 C2 P 111.8(3) . . ?
N2 C2 H21 109.3 . . ?
P C2 H21 109.3 . . ?
N2 C2 H22 109.3 . . ?
P C2 H22 109.3 . . ?
H21 C2 H22 107.9 . . ?
N3 C3 P 110.5(3) . . ?
N3 C3 H31 109.5 . . ?
P C3 H31 109.5 . . ?
N3 C3 H32 109.5 . . ?
P C3 H32 109.5 . . ?
H31 C3 H32 108.1 . . ?
N1 C4 H41 109.5 . . ?
N1 C4 H42 109.5 . . ?
H41 C4 H42 109.5 . . ?
N1 C4 H43 109.5 . . ?
H41 C4 H43 109.5 . . ?
H42 C4 H43 109.5 . . ?
N2 C5 N1 111.9(3) . . ?
N2 C5 H51 109.2 . . ?
N1 C5 H51 109.2 . . ?
N2 C5 H52 109.2 . . ?
N1 C5 H52 109.2 . . ?
H51 C5 H52 107.9 . . ?
N3 C6 N1 111.6(4) . . ?
N3 C6 H61 109.3 . . ?
N1 C6 H61 109.3 . . ?
N3 C6 H62 109.3 . . ?
N1 C6 H62 109.3 . . ?
H61 C6 H62 108.0 . . ?
N2 C7 N3 112.5(4) . . ?
N2 C7 H71 109.1 . . ?
N3 C7 H71 109.1 . . ?
N2 C7 H72 109.1 . . ?
N3 C7 H72 109.1 . . ?
H71 C7 H72 107.8 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh P 2.3179(13) . ?
Rh P 2.3179(13) 3_666 ?
Rh I2 2.6837(9) 3_666 ?
Rh I2 2.6837(9) . ?
Rh I1 2.7006(9) . ?
Rh I1 2.7006(9) 3_666 ?
I3 I31 0.67(4) . ?
I3 I3 2.940(6) 3_767 ?
P C1 1.840(5) . ?
P C2 1.842(5) . ?
P C3 1.854(5) . ?
N1 C4 1.494(5) . ?
N1 C1 1.512(6) . ?
N1 C6 1.527(6) . ?
N1 C5 1.540(5) . ?
N2 C5 1.429(5) . ?
N2 C7 1.462(7) . ?
N2 C2 1.479(6) . ?
N3 C6 1.432(6) . ?
N3 C7 1.465(7) . ?
N3 C3 1.475(6) . ?
C1 H11 0.9900 . ?
C1 H12 0.9900 . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
C4 H41 0.9800 . ?
C4 H42 0.9800 . ?
C4 H43 0.9800 . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
C7 H71 0.9900 . ?
C7 H72 0.9900 . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P Rh P C1 -160(100) 3_666 . . . ?
I2 Rh P C1 53.98(17) 3_666 . . . ?
I2 Rh P C1 -126.02(17) . . . . ?
I1 Rh P C1 -35.33(17) . . . . ?
I1 Rh P C1 144.67(17) 3_666 . . . ?
P Rh P C2 82(100) 3_666 . . . ?
I2 Rh P C2 -63.66(19) 3_666 . . . ?
I2 Rh P C2 116.34(19) . . . . ?
I1 Rh P C2 -152.98(19) . . . . ?
I1 Rh P C2 27.02(19) 3_666 . . . ?
P Rh P C3 -41(100) 3_666 . . . ?
I2 Rh P C3 172.83(19) 3_666 . . . ?
I2 Rh P C3 -7.17(19) . . . . ?
I1 Rh P C3 83.51(19) . . . . ?
I1 Rh P C3 -96.49(19) 3_666 . . . ?
C4 N1 C1 P 179.5(3) . . . . ?
C6 N1 C1 P -60.6(4) . . . . ?
C5 N1 C1 P 58.7(4) . . . . ?
C2 P C1 N1 -48.7(3) . . . . ?
C3 P C1 N1 51.2(3) . . . . ?
Rh P C1 N1 -177.1(2) . . . . ?
C5 N2 C2 P -63.6(5) . . . . ?
C7 N2 C2 P 61.1(5) . . . . ?
C1 P C2 N2 49.4(4) . . . . ?
C3 P C2 N2 -49.4(4) . . . . ?
Rh P C2 N2 176.2(3) . . . . ?
C6 N3 C3 P 65.2(5) . . . . ?
C7 N3 C3 P -60.8(4) . . . . ?
C1 P C3 N3 -51.3(4) . . . . ?
C2 P C3 N3 48.5(4) . . . . ?
Rh P C3 N3 -179.0(2) . . . . ?
C7 N2 C5 N1 -56.7(4) . . . . ?
C2 N2 C5 N1 69.0(4) . . . . ?
C4 N1 C5 N2 173.6(2) . . . . ?
C1 N1 C5 N2 -66.0(4) . . . . ?
C6 N1 C5 N2 54.5(4) . . . . ?
C7 N3 C6 N1 57.7(5) . . . . ?
C3 N3 C6 N1 -70.0(5) . . . . ?
C4 N1 C6 N3 -174.2(4) . . . . ?
C1 N1 C6 N3 66.1(5) . . . . ?
C5 N1 C6 N3 -54.9(5) . . . . ?
C5 N2 C7 N3 58.9(5) . . . . ?
C2 N2 C7 N3 -67.5(5) . . . . ?
C6 N3 C7 N2 -59.4(5) . . . . ?
C3 N3 C7 N2 68.3(5) . . . . ?
