#------------------------------------------------------------------------------
#$Date: 2017-02-10 18:21:58 +0200 (Fri, 10 Feb 2017) $
#$Revision: 191977 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/38/2003856.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_2003856
loop_
_publ_author_name
'Ertan, A.'
'Adolfsson, H.'
'Moberg, C.'
_publ_section_title
;
 Trichloro[tris(2-pyridyl)methanol]rhodium(III)--Methanol (1/1)
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1761
_journal_page_last               1765
_journal_paper_doi               10.1107/S0108270195002939
_journal_volume                  51
_journal_year                    1995
_chemical_compound_source        'Adolfsson et al.'
_chemical_formula_moiety         'C16 H13 Cl3 N3 O Rh1 , C H4 O'
_chemical_formula_structural     '[Rh(C16H13N3OCl3)].CH3OH'
_chemical_formula_sum            'C17 H17 Cl3 N3 O2 Rh'
_chemical_formula_weight         504.605
_chemical_name_systematic
;
 trichloro[tris(2-pyridyl)methanol]rhodium(III).MeOH
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 102.43(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3218(5)
_cell_length_b                   15.1916(12)
_cell_length_c                   14.9796(9)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      17.2
_cell_measurement_theta_min      10.5
_cell_volume                     1849.4(2)
_computing_data_collection       'DIF4 (Stoe & Cie, 1988a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1988b)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1990)'
_computing_publication_material  'PARST (Nardelli, 1983)'
_computing_structure_refinement  'SHELX76 (Sheldrick, 1976)'
_computing_structure_solution    'DIRDIF (Beurskens et al., 1992)'
_diffrn_ambient_temperature      153(2)
_diffrn_measurement_device       'Siemens STOE AED2'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8814
_diffrn_reflns_theta_max         34.995
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    1.249
_exptl_absorpt_correction_T_max  0.847
_exptl_absorpt_correction_T_min  0.797
_exptl_absorpt_correction_type   'numerical integration (Norrestam, 1989)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.8123(2)
_exptl_crystal_description       plate
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         .240
_refine_diff_density_min         -.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   'not given by SHELX76'
_refine_ls_hydrogen_treatment    'H atoms refined using riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3514
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.
_refine_ls_R_factor_obs          0.0301
_refine_ls_shift/esd_max         0.016
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[s²(F) + 0.0002F²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.
_refine_ls_wR_factor_obs         0.0334
_reflns_number_observed          3514
_reflns_number_total             8105
_reflns_observed_criterion       I>3\s(I)
_cod_data_source_file            ab1264.cif
_cod_data_source_block           rhcomp
_cod_depositor_comments
;
 Changing the _atom_site_occupancy data item value from '.' to '1'
 for all fully occupied atom sites.

 Antanas Vaitkus,
 2017-02-10

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w = 1/[s^2^(F) +
0.0002F^2^]' 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^(F) + 0.0002F^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1849.39(23)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C17 H17 Cl3 N3 O2 Rh1'
_cod_database_code               2003856
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x+1/2, -y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_occupancy
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_type_symbol
Rh 1 0.06971(3) 0.23270(2) 0.07570(2) 0.0149(1) Uani d Rh
Cl1 1 -0.1562(1) 0.1473(1) 0.0018(1) 0.0237(3) Uani d Cl
Cl2 1 -0.0866(1) 0.3043(1) 0.1684(1) 0.0235(3) Uani d Cl
Cl3 1 0.1483(1) 0.1232(1) 0.1872(1) 0.0277(3) Uani d Cl
N1 1 0.0029(4) 0.3287(2) -0.0192(2) 0.0163(8) Uani d N
C2 1 0.1201(4) 0.3706(2) -0.0523(2) 0.0158(9) Uani d C
C3 1 0.0846(4) 0.4458(2) -0.1063(2) 0.0196(10) Uani d C
H3 1 0.1784(4) 0.4769(2) -0.1264(2) 0.024(11) Uiso d H
C4 1 -0.0789(5) 0.4749(2) -0.1294(2) 0.0237(11) Uani d C
H4 1 -0.0991(5) 0.5249(2) -0.1674(2) 0.032(12) Uiso d H
C5 1 -0.2001(5) 0.4291(2) -0.0984(2) 0.0218(10) Uani d C
H5 1 -0.3201(5) 0.4410(2) -0.1118(2) 0.029(12) Uiso d H
C6 1 -0.1555(4) 0.3570(2) -0.0426(2) 0.0192(10) Uani d C
H6 1 -0.2357(4) 0.3208(2) -0.0194(2) 0.024(11) Uiso d H
C1 1 0.2976(4) 0.3335(2) -0.0250(2) 0.0161(9) Uani d C
O1 1 0.4036(3) 0.3802(2) -0.0696(2) 0.0209(8) Uani d O
H1O 1 0.3513(3) 0.3759(2) -0.1364(2) 0.062(17) Uiso d H
C2" 1 0.3048(4) 0.2337(2) -0.0448(2) 0.0169(8) Uani d C
C3" 1 0.4098(4) 0.2009(2) -0.0982(2) 0.0191(10) Uani d C
H3" 1 0.4852(4) 0.2443(2) -0.1263(2) 0.034(13) Uiso d H
C4" 1 0.4181(5) 0.1094(2) -0.1105(2) 0.0239(11) Uani d C
H4" 1 0.4999(5) 0.0827(2) -0.1486(2) 0.0173(98) Uiso d H
C5" 1 0.3226(5) 0.0548(2) -0.0692(2) 0.0230(11) Uani d C
H5" 1 0.3216(5) -0.0090(2) -0.0746(2) 0.052(15) Uiso d H
C6" 1 0.2202(4) 0.0907(2) -0.0165(2) 0.0202(10) Uani d C
H6" 1 0.1483(4) 0.0564(2) 0.0140(2) 0.0149(94) Uiso d H
N1" 1 0.2130(3) 0.1788(2) -0.0043(2) 0.0170(8) Uani d N
N1' 1 0.2697(4) 0.3073(2) 0.1335(2) 0.0181(8) Uani d N
C2' 1 0.3587(4) 0.3477(2) 0.0790(2) 0.0174(9) Uani d C
C3' 1 0.4951(4) 0.4002(2) 0.1149(2) 0.0224(11) Uani d C
H3' 1 0.5408(4) 0.4247(2) 0.0656(2) 0.0154(97) Uiso d H
C4' 1 0.5363(5) 0.4148(3) 0.2087(3) 0.0275(12) Uani d C
H4' 1 0.6284(5) 0.4558(3) 0.2356(3) 0.023(10) Uiso d H
C5' 1 0.4435(5) 0.3742(2) 0.2645(2) 0.0262(11) Uani d C
H5' 1 0.4553(5) 0.3837(2) 0.3235(2) 0.0066(83) Uiso d H
C6' 1 0.3124(4) 0.3211(2) 0.2258(2) 0.0224(10) Uani d C
H6' 1 0.2456(4) 0.2942(2) 0.2637(2) 0.0141(95) Uiso d H
C1M 1 0.1248(6) 0.3465(3) -0.3006(3) 0.0352(14) Uani d C
H1M 1 0.0346(6) 0.3847(3) -0.2877(3) 0.074(19) Uiso d H
H2M 1 0.1144(6) 0.3417(3) -0.3622(3) 0.035(12) Uiso d H
H3M 1 0.1163(6) 0.2866(3) -0.2744(3) 0.083(21) Uiso d H
O1M 1 0.2812(4) 0.3847(2) -0.2558(2) 0.0278(9) Uani d O
H1OM 1 0.3550(4) 0.3565(2) -0.2770(2) 0.032(3) Uiso d H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_source
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
C C 'International Tables 1974 Vol IV Table 2.2B' .002 .002
H H 'International Tables 1974 Vol IV Table 2.2B' .0000 .0000
O O 'International Tables 1974 Vol IV Table 2.2B' .008 .006
Cl Cl 'International Tables 1974 Vol IV Table 2.2B' .132 .159
N N 'International Tables 1974 Vol IV Table 2.2B' .002 .002
Rh Rh 'International Tables 1974 Vol IV Table 2.2B' -1.287 .919
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
N1" Rh N1' 86.90(10) yes
N1 Rh N1' 88.50(10) yes
N1 Rh N1" 89.10(10) yes
Cl3 Rh N1' 90.80(10) yes
Cl3 Rh N1" 91.40(10) yes
Cl3 Rh N1 179.20(10) yes
Cl2 Rh N1' 89.80(10) yes
Cl2 Rh N1" 176.10(10) yes
Cl2 Rh N1 88.70(10) yes
Cl2 Rh Cl3 90.70(10) yes
Cl1 Rh N1' 177.00(10) yes
Cl1 Rh N1" 90.60(10) yes
Cl1 Rh N1 89.80(10) yes
Cl1 Rh Cl3 90.90(10) yes
Cl1 Rh Cl2 92.60(10) yes
Rh N1 C6 120.8(2) ?
Rh N1 C2 119.1(2) ?
C2 N1 C6 119.7(3) ?
N1 C2 C1 117.1(3) yes
N1 C2 C3 121.4(3) ?
C3 C2 C1 121.4(3) ?
C2 C3 C4 118.4(3) ?
C3 C4 C5 119.8(3) ?
C4 C5 C6 118.8(4) ?
N1 C6 C5 121.8(3) ?
C2 C1 C2' 107.6(3) yes
C2 C1 C2" 112.3(3) yes
C2 C1 O1 110.5(3) yes
C2" C1 C2' 108.1(3) yes
O1 C1 C2' 107.7(3) yes
O1 C1 C2" 110.4(3) yes
C1 C2" N1" 117.8(3) yes
C1 C2" C3" 120.9(3) ?
C3" C2" N1" 121.2(3) ?
C2" C3" C4" 118.8(3) ?
C3" C4" C5" 119.0(3) ?
C4" C5" C6" 120.0(3) ?
C5" C6" N1" 121.0(3) ?
C2" N1" C6" 120.0(3) ?
Rh N1" C6" 121.7(2) ?
Rh N1" C2" 118.2(2) ?
Rh N1' C6' 121.6(2) ?
Rh N1' C2' 119.6(2) ?
C2' N1' C6' 118.7(3) ?
C1 C2' N1' 116.0(3) yes
N1' C2' C3' 121.9(3) ?
C1 C2' C3' 122.1(3) ?
C2' C3' C4' 118.9(3) ?
C3' C4' C5' 119.1(4) ?
C4' C5' C6' 119.6(3) ?
N1' C6' C5' 121.7(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Rh Cl1 2.3557(9) yes
Rh Cl2 2.3625(10) yes
Rh Cl3 2.3482(9) yes
Rh N1 2.030(3) yes
Rh N1" 2.035(3) yes
Rh N1' 2.046(3) yes
Cl1 Cl3 3.3530(10) yes
Cl1 N1 3.103(3) yes
Cl3 N1' 3.137(3) yes
N1 N1' 2.844(4) yes
Cl1 N1" 3.130(3) yes
Cl2 Cl3 3.3520(10) yes
Cl2 N1 3.081(3) yes
Cl2 N1' 3.119(3) yes
Cl3 N1" 3.145(3) yes
N1 N1" 2.851(4) yes
N1" N1' 2.807(4) yes
Cl1 Cl2 3.4110(10) yes
N1 C2 1.345(5) ?
N1 C6 1.359(4) ?
C2 C3 1.394(5) ?
C2 C1 1.551(5) yes
C3 C4 1.402(5) ?
C4 C5 1.385(6) ?
C5 C6 1.379(5) ?
C1 O1 1.407(4) yes
C1 C2" 1.549(5) yes
C1 C2' 1.546(4) yes
C2" C3" 1.397(5) ?
C2" N1" 1.359(5) ?
C3" C4" 1.406(5) ?
C4" C5" 1.383(6) ?
C5" C6" 1.392(6) ?
C6" N1" 1.354(4) ?
N1' C2' 1.361(5) ?
N1' C6' 1.366(4) ?
C2' C3' 1.396(5) ?
C3' C4' 1.390(5) ?
C4' C5' 1.398(6) ?
C5' C6' 1.380(5) ?
C1M O1M 1.451(5) yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Cl2 C1M 3.423(5) 4_455 yes
Cl3 C4 3.499(4) 4 yes
Cl3 C5 3.285(4) 4 yes
O1 C5 3.497(5) 1_655 yes
O1M C3 3.183(5) . yes
O1M C4' 3.410(5) 3_665 yes
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_publ_flag
N1" Rh N1' C2' 45.5(3) ?
N1 Rh N1' C2' -43.7(3) ?
Cl3 Rh N1' C2' 136.8(2) ?
Cl2 Rh N1' C2' -132.4(2) ?
N1" Rh N1' C6' -137.5(3) ?
N1 Rh N1' C6' 133.4(3) ?
Cl3 Rh N1' C6' -46.1(3) ?
Cl2 Rh N1' C6' 44.6(3) ?
N1' Rh N1" C2" -46.1(3) ?
N1 Rh N1" C2" 42.4(2) ?
Cl3 Rh N1" C2" -136.9(2) ?
Cl1 Rh N1" C2" 132.2(2) ?
N1' Rh N1" C6" 132.9(3) ?
N1 Rh N1" C6" -138.6(3) ?
Cl3 Rh N1" C6" 42.1(3) ?
Cl1 Rh N1" C6" -48.8(3) ?
Cl2 Rh N1 C2 128.5(2) ?
Cl1 Rh N1 C2 -138.9(2) ?
Cl2 Rh N1 C6 -44.8(2) ?
Cl1 Rh N1 C6 47.8(2) ?
N1" Rh N1 C6 138.4(3) ?
N1" Rh N1 C2 -48.3(3) ?
N1' Rh N1 C6 -134.6(3) ?
N1' Rh N1 C2 38.7(3) ?
Rh N1 C6 C5 172.0(3) ?
Rh N1 C2 C3 -169.8(3) ?
Rh N1 C2 C1 8.2(4) ?
C2 N1 C6 C5 -1.2(5) ?
C6 N1 C2 C1 -178.4(3) ?
C6 N1 C2 C3 3.5(5) ?
N1 C2 C1 O1 175.9(3) yes
N1 C2 C1 C2" 52.2(4) yes
N1 C2 C1 C2' -66.7(4) yes
N1 C2 C3 C4 -2.9(5) ?
C3 C2 C1 O1 -6.0(4) yes
C3 C2 C1 C2" -129.8(3) yes
C3 C2 C1 C2' 111.4(4) yes
C1 C2 C3 C4 179.2(3) ?
C2 C3 C4 C5 -.1(5) ?
C3 C4 C5 C6 2.2(6) ?
C4 C5 C6 N1 -1.7(6) ?
C2 C1 C2' C3' -118.2(4) yes
C2 C1 C2' N1' 60.5(4) yes
C2 C1 C2" C3" 125.5(4) yes
C2 C1 C2" N1" -58.2(4) yes
C2" C1 C2' C3' 120.3(4) yes
O1 C1 C2' C3' 1.0(4) yes
C2" C1 C2' N1' -61.0(4) yes
O1 C1 C2' N1' 179.7(3) yes
O1 C1 C2" C3" 1.7(4) yes
O1 C1 C2" N1" 178.0(3) yes
C2' C1 C2" N1" 60.4(4) yes
C2' C1 C2" C3" -115.9(4) yes
C1 C2" N1" Rh 1.6(4) ?
C3" C2" N1" Rh 178.0(3) ?
C1 C2" N1" C6" -177.4(3) ?
C1 C2" C3" C4" 176.9(3) ?
C3" C2" N1" C6" -1.0(5) ?
N1" C2" C3" C4" .6(5) ?
C2" C3" C4" C5" -.2(5) ?
C3" C4" C5" C6" .1(6) ?
C4" C5" C6" N1" -.4(6) ?
C5" C6" N1" C2" .9(5) ?
C5" C6" N1" Rh -178.1(3) ?
Rh N1' C2' C1 .5(4) ?
Rh N1' C6' C5' -177.5(3) ?
Rh N1' C2' C3' 179.2(3) ?
C6' N1' C2' C1 -176.6(3) ?
C2' N1' C6' C5' -.4(5) ?
C6' N1' C2' C3' 2.1(5) ?
N1' C2' C3' C4' -2.9(5) ?
C1 C2' C3' C4' 175.7(3) ?
C2' C3' C4' C5' 2.0(6) ?
C3' C4' C5' C6' -.5(6) ?
C4' C5' C6' N1' -.4(6) ?
