#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:35:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179337 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/34/4323481.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_4323481
loop_
_publ_author_name
'Jaap W. van Hal'
'Lawrence B. Alemany'
'Kenton H. Whitmire'
_publ_contact_author
; 
Dr. Kenton. H. Whitmire
Chemistry Department MS 60
Rice University
6100 Main Street
Houston TX 77005-1892
U.S.A.
;
_publ_contact_author_email       whitmir@rice.edu
_publ_contact_author_fax         (1)-713-737-5652
_publ_contact_author_phone       (1)-713-737-5650
_publ_section_title
;
 Solution Dynamics of Thallium-Metal Carbonyl Compounds Using 205Tl NMR
 Spectroscopy
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3152
_journal_page_last               3159
_journal_paper_doi               10.1021/ic961203k
_journal_volume                  36
_journal_year                    1997
_chemical_formula_moiety
; 
'C28 H32 Fe3 N4 O12 Tl2'
;
_chemical_formula_structural
;
((CH3)2CNCH2CH2NC(CH3)2TlFe(CO)4)2Fe(CO)4
;
_chemical_formula_sum            'C28 H32 Fe3 N4 O12 Tl2'
_chemical_formula_weight         1192.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           primitive
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                92.75(3)
_cell_angle_beta                 95.07(3)
_cell_angle_gamma                114.40(3)
_cell_formula_units_Z            2
_cell_length_a                   13.597(3)
_cell_length_b                   15.040(3)
_cell_length_c                   10.536(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      6
_cell_measurement_theta_min      3
_cell_volume                     1946.0(9)
_computing_cell_refinement       'TEXSAN 5.0'
_computing_data_collection       'TEXSAN 5.0'
_computing_data_reduction        'TEXSAN 5.0'
_computing_molecular_graphics    SHELXTL-PLUS
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku AFC5-S'
_diffrn_measurement_method       ω-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3867
_diffrn_reflns_theta_max         22.46
_diffrn_reflns_theta_min         2.34
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.402
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  .1481
_exptl_absorpt_correction_type   emperical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.036
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .4
_exptl_crystal_size_min          .5
_refine_diff_density_max         1.943
_refine_diff_density_min         -2.722
_refine_diff_density_rms         0.323
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.142
_refine_ls_goodness_of_fit_obs   1.173
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         3659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_restrained_S_obs      1.173
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_obs          0.0461
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0922P)²+3.6895P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1377
_refine_ls_wR_factor_obs         0.1295
_reflns_number_observed          3163
_reflns_number_total             3660
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961203k_1.cif
_cod_data_source_block           ltl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'no-ref' changed to 'noref'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0922P)^2^+3.6895P] 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^)+(0.0922P)^2^+3.6895P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1946.0(7)
_cod_database_code               4323481
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Tl1 Tl 0.31560(4) 0.15020(4) 0.25224(5) 0.0494(3) Uani 1 d . .
Tl2 Tl 0.09905(4) 0.28272(4) 0.26273(5) 0.0462(3) Uani 1 d . .
Fe1 Fe 0.5181(2) 0.2590(2) 0.3266(2) 0.0586(6) Uani 1 d . .
Fe2 Fe -0.0381(2) 0.3407(2) 0.1546(2) 0.0592(6) Uani 1 d . .
Fe3 Fe 0.1057(2) 0.10378(15) 0.2842(2) 0.0509(6) Uani 1 d . .
C11 C 0.6591(18) 0.3220(15) 0.3874(18) 0.082(5) Uani 1 d . .
O11 O 0.7469(12) 0.3623(12) 0.4256(14) 0.115(5) Uani 1 d . .
C12 C 0.5399(15) 0.1730(14) 0.2283(22) 0.090(6) Uani 1 d . .
O12 O 0.5550(13) 0.1154(14) 0.1717(20) 0.160(8) Uani 1 d . .
C13 C 0.5171(14) 0.3557(14) 0.2439(17) 0.072(5) Uani 1 d . .
O13 O 0.5214(11) 0.4225(11) 0.1884(15) 0.099(4) Uani 1 d . .
C14 C 0.4798(15) 0.2525(14) 0.4834(21) 0.083(6) Uani 1 d . .
O14 O 0.4605(12) 0.2513(12) 0.5877(14) 0.109(5) Uani 1 d . .
C21 C -0.0192(15) 0.3004(14) 0.0026(20) 0.082(6) Uani 1 d . .
O21 O -0.0105(12) 0.2733(12) -0.1027(12) 0.112(5) Uani 1 d . .
C22 C -0.1370(16) 0.2545(13) 0.2412(16) 0.065(5) Uani 1 d . .
O22 O -0.2001(11) 0.1976(11) 0.2903(14) 0.098(4) Uani 1 d . .
C23 C 0.0550(19) 0.4586(17) 0.2232(21) 0.091(6) Uani 1 d . .
O23 O 0.1121(13) 0.5368(11) 0.2660(16) 0.115(5) Uani 1 d . .
C24 C -0.1303(18) 0.3800(16) 0.0897(21) 0.095(6) Uani 1 d . .
O24 O -0.1966(18) 0.4006(16) 0.0492(19) 0.159(7) Uani 1 d . .
C31 C -0.0297(17) 0.0695(14) 0.3118(22) 0.092(7) Uani 1 d . .
O31 O -0.1161(14) 0.0434(13) 0.3356(21) 0.151(8) Uani 1 d . .
C32 C 0.0860(13) -0.0252(15) 0.2931(16) 0.067(5) Uani 1 d . .
O32 O 0.0646(12) -0.1033(9) 0.3036(15) 0.104(5) Uani 1 d . .
C33 C 0.0956(13) 0.1094(11) 0.1146(18) 0.061(4) Uani 1 d . .
O33 O 0.0834(10) 0.1109(9) 0.0057(12) 0.082(4) Uani 1 d . .
C34 C 0.1689(14) 0.1517(12) 0.4463(17) 0.061(4) Uani 1 d . .
O34 O 0.2010(12) 0.1756(10) 0.5498(12) 0.091(4) Uani 1 d . .
N41 N 0.3017(11) 0.0771(9) 0.0249(12) 0.059(3) Uani 1 d . .
N42 N 0.3052(10) -0.0289(9) 0.2453(12) 0.060(4) Uani 1 d . .
C41 C 0.3897(22) 0.2264(15) -0.0614(19) 0.132(10) Uani 1 d . .
H41A H 0.3737(22) 0.2517(15) 0.0157(19) 0.198 Uiso 1 calc R .
H41B H 0.3564(22) 0.2441(15) -0.1342(19) 0.198 Uiso 1 calc R .
H41C H 0.4670(22) 0.2535(15) -0.0630(19) 0.198 Uiso 1 calc R .
C42 C 0.3692(18) 0.0752(17) -0.1838(18) 0.117(8) Uani 1 d . .
H42A H 0.3394(18) 0.0053(17) -0.1813(18) 0.175 Uiso 1 calc R .
H42B H 0.4462(18) 0.1001(17) -0.1871(18) 0.175 Uiso 1 calc R .
H42C H 0.3357(18) 0.0907(17) -0.2584(18) 0.175 Uiso 1 calc R .
C43 C 0.3476(14) 0.1215(12) -0.0653(15) 0.066(5) Uani 1 d . .
C44 C 0.2468(21) -0.0313(12) 0.0221(19) 0.108(8) Uani 1 d . .
H44A H 0.1704(21) -0.0501(12) 0.0297(19) 0.130 Uiso 1 calc R .
H44B H 0.2515(21) -0.0595(12) -0.0608(19) 0.130 Uiso 1 calc R .
C45 C 0.2878(19) -0.0721(13) 0.1159(17) 0.088(6) Uani 1 d . .
H45A H 0.3567(19) -0.0693(13) 0.0936(17) 0.106 Uiso 1 calc R .
H45B H 0.2385(19) -0.1408(13) 0.1137(17) 0.106 Uiso 1 calc R .
C46 C 0.3159(14) -0.0721(12) 0.3402(20) 0.075(5) Uani 1 d . .
C47 C 0.3124(23) -0.1765(16) 0.3283(24) 0.137(10) Uani 1 d . .
H47A H 0.3034(23) -0.1992(16) 0.2396(24) 0.205 Uiso 1 calc R .
H47B H 0.2525(23) -0.2201(16) 0.3687(24) 0.205 Uiso 1 calc R .
H47C H 0.3791(23) -0.1748(16) 0.3694(24) 0.205 Uiso 1 calc R .
C48 C 0.3297(19) -0.0252(17) 0.4731(17) 0.109(8) Uani 1 d . .
H48A H 0.3307(19) 0.0389(17) 0.4691(17) 0.163 Uiso 1 calc R .
H48B H 0.3969(19) -0.0194(17) 0.5180(17) 0.163 Uiso 1 calc R .
H48C H 0.2703(19) -0.0648(17) 0.5174(17) 0.163 Uiso 1 calc R .
N51 N 0.2877(10) 0.4178(10) 0.2576(12) 0.060(4) Uani 1 d . .
N52 N 0.1784(11) 0.3671(9) 0.4788(11) 0.058(3) Uani 1 d . .
C51 C 0.2702(15) 0.4050(14) 0.0295(16) 0.084(6) Uani 1 d . .
H51A H 0.2211(15) 0.3389(14) 0.0401(16) 0.126 Uiso 1 calc R .
H51B H 0.3273(15) 0.4043(14) -0.0174(16) 0.126 Uiso 1 calc R .
H51C H 0.2314(15) 0.4364(14) -0.0166(16) 0.126 Uiso 1 calc R .
C52 C 0.3965(16) 0.5644(14) 0.1567(21) 0.102(7) Uani 1 d . .
H52A H 0.4221(16) 0.5925(14) 0.2435(21) 0.152 Uiso 1 calc R .
H52B H 0.3610(16) 0.6001(14) 0.1140(21) 0.152 Uiso 1 calc R .
H52C H 0.4570(16) 0.5680(14) 0.1132(21) 0.152 Uiso 1 calc R .
C53 C 0.3173(13) 0.4590(11) 0.1556(17) 0.062(4) Uani 1 d . .
C54 C 0.2958(16) 0.4113(14) 0.4852(15) 0.083(6) Uani 1 d . .
H54A H 0.3214(16) 0.3600(14) 0.4794(15) 0.100 Uiso 1 calc R .
H54B H 0.3266(16) 0.4494(14) 0.5673(15) 0.100 Uiso 1 calc R .
C55 C 0.3351(15) 0.4770(13) 0.3796(15) 0.081(5) Uani 1 d . .
H55A H 0.3127(15) 0.5303(13) 0.3865(15) 0.097 Uiso 1 calc R .
H55B H 0.4138(15) 0.5047(13) 0.3858(15) 0.097 Uiso 1 calc R .
C56 C 0.1245(19) 0.3674(12) 0.5730(15) 0.081(6) Uani 1 d . .
C57 C 0.1776(23) 0.4159(22) 0.7036(19) 0.173(15) Uani 1 d . .
H57A H 0.2550(23) 0.4468(22) 0.7032(19) 0.260 Uiso 1 calc R .
H57B H 0.1597(23) 0.3676(22) 0.7643(19) 0.260 Uiso 1 calc R .
H57C H 0.1520(23) 0.4644(22) 0.7271(19) 0.260 Uiso 1 calc R .
C58 C 0.0038(15) 0.3151(16) 0.5542(18) 0.092(6) Uani 1 d . .
H58A H -0.0201(15) 0.2875(16) 0.4670(18) 0.139 Uiso 1 calc R .
H58B H -0.0272(15) 0.3604(16) 0.5733(18) 0.139 Uiso 1 calc R .
H58C H -0.0194(15) 0.2636(16) 0.6102(18) 0.139 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tl Tl -2.8358 9.6688 '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
N41 Tl1 Fe1 107.7(3) . . ?
N41 Tl1 N42 67.7(4) . . ?
Fe1 Tl1 N42 103.3(3) . . ?
N41 Tl1 Fe3 102.7(3) . . ?
Fe1 Tl1 Fe3 147.91(7) . . ?
N42 Tl1 Fe3 97.5(3) . . ?
N52 Tl2 N51 69.1(4) . . ?
N52 Tl2 Fe2 112.7(3) . . ?
N51 Tl2 Fe2 107.4(3) . . ?
N52 Tl2 Fe3 102.0(3) . . ?
N51 Tl2 Fe3 111.5(3) . . ?
Fe2 Tl2 Fe3 134.95(8) . . ?
C13 Fe1 C12 111.8(9) . . ?
C13 Fe1 C14 117.5(9) . . ?
C12 Fe1 C14 130.1(10) . . ?
C13 Fe1 C11 93.8(9) . . ?
C12 Fe1 C11 93.1(8) . . ?
C14 Fe1 C11 91.3(8) . . ?
C13 Fe1 Tl1 93.1(6) . . ?
C12 Fe1 Tl1 83.9(6) . . ?
C14 Fe1 Tl1 85.9(6) . . ?
C11 Fe1 Tl1 173.0(7) . . ?
C24 Fe2 C21 91.9(10) . . ?
C24 Fe2 C23 94.4(10) . . ?
C21 Fe2 C23 117.9(9) . . ?
C24 Fe2 C22 91.9(9) . . ?
C21 Fe2 C22 118.5(8) . . ?
C23 Fe2 C22 123.0(9) . . ?
C24 Fe2 Tl2 177.4(8) . . ?
C21 Fe2 Tl2 90.6(6) . . ?
C23 Fe2 Tl2 84.8(6) . . ?
C22 Fe2 Tl2 86.6(6) . . ?
C31 Fe3 C33 101.2(9) . . ?
C31 Fe3 C34 97.9(9) . . ?
C33 Fe3 C34 153.0(7) . . ?
C31 Fe3 C32 89.3(8) . . ?
C33 Fe3 C32 100.5(7) . . ?
C34 Fe3 C32 98.7(7) . . ?
C31 Fe3 Tl1 176.7(7) . . ?
C33 Fe3 Tl1 81.5(5) . . ?
C34 Fe3 Tl1 80.2(5) . . ?
C32 Fe3 Tl1 88.3(5) . . ?
C31 Fe3 Tl2 82.1(6) . . ?
C33 Fe3 Tl2 78.1(5) . . ?
C34 Fe3 Tl2 85.8(5) . . ?
C32 Fe3 Tl2 170.7(5) . . ?
Tl1 Fe3 Tl2 100.44(7) . . ?
O11 C11 Fe1 179.2(18) . . ?
O12 C12 Fe1 175.8(23) . . ?
O13 C13 Fe1 177.0(16) . . ?
O14 C14 Fe1 176.4(16) . . ?
O21 C21 Fe2 177.1(17) . . ?
O22 C22 Fe2 176.7(16) . . ?
O23 C23 Fe2 176.9(18) . . ?
O24 C24 Fe2 175.4(23) . . ?
O31 C31 Fe3 175.3(19) . . ?
O32 C32 Fe3 172.7(16) . . ?
O33 C33 Fe3 176.5(16) . . ?
O34 C34 Fe3 174.5(15) . . ?
C43 N41 C44 123.9(14) . . ?
C43 N41 Tl1 126.7(10) . . ?
C44 N41 Tl1 108.4(10) . . ?
C46 N42 C45 122.8(15) . . ?
C46 N42 Tl1 125.7(12) . . ?
C45 N42 Tl1 111.4(10) . . ?
N41 C43 C41 121.0(16) . . ?
N41 C43 C42 125.8(16) . . ?
C41 C43 C42 113.1(16) . . ?
C45 C44 N41 115.5(17) . . ?
C44 C45 N42 117.4(16) . . ?
N42 C46 C48 120.6(16) . . ?
N42 C46 C47 122.8(19) . . ?
C48 C46 C47 116.6(17) . . ?
C53 N51 C55 117.5(13) . . ?
C53 N51 Tl2 121.7(10) . . ?
C55 N51 Tl2 113.8(9) . . ?
C56 N52 C54 125.0(14) . . ?
C56 N52 Tl2 125.6(12) . . ?
C54 N52 Tl2 109.3(9) . . ?
N51 C53 C51 120.4(14) . . ?
N51 C53 C52 123.0(16) . . ?
C51 C53 C52 116.5(16) . . ?
N52 C54 C55 112.1(14) . . ?
N51 C55 C54 107.9(14) . . ?
N52 C56 C58 119.3(15) . . ?
N52 C56 C57 123.1(20) . . ?
C58 C56 C57 117.6(18) . . ?
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
Tl1 N41 2.545(12) . ?
Tl1 Fe1 2.578(2) . ?
Tl1 N42 2.635(13) . ?
Tl1 Fe3 2.700(2) . ?
Tl2 N52 2.472(12) . ?
Tl2 N51 2.538(13) . ?
Tl2 Fe2 2.569(2) . ?
Tl2 Fe3 2.749(2) . ?
Fe1 C13 1.73(2) . ?
Fe1 C12 1.75(2) . ?
Fe1 C14 1.77(2) . ?
Fe1 C11 1.79(2) . ?
Fe2 C24 1.70(2) . ?
Fe2 C21 1.76(2) . ?
Fe2 C23 1.77(2) . ?
Fe2 C22 1.79(2) . ?
Fe3 C31 1.75(2) . ?
Fe3 C33 1.79(2) . ?
Fe3 C34 1.81(2) . ?
Fe3 C32 1.85(2) . ?
C11 O11 1.12(2) . ?
C12 O12 1.13(2) . ?
C13 O13 1.17(2) . ?
C14 O14 1.15(2) . ?
C21 O21 1.20(2) . ?
C22 O22 1.12(2) . ?
C23 O23 1.15(2) . ?
C24 O24 1.13(2) . ?
C31 O31 1.13(2) . ?
C32 O32 1.10(2) . ?
C33 O33 1.15(2) . ?
C34 O34 1.12(2) . ?
N41 C43 1.25(2) . ?
N41 C44 1.48(2) . ?
N42 C46 1.25(2) . ?
N42 C45 1.44(2) . ?
C41 C43 1.44(2) . ?
C42 C43 1.51(2) . ?
C44 C45 1.38(3) . ?
C46 C48 1.50(3) . ?
C46 C47 1.55(3) . ?
N51 C53 1.28(2) . ?
N51 C55 1.46(2) . ?
N52 C56 1.29(2) . ?
N52 C54 1.45(2) . ?
C51 C53 1.47(2) . ?
C52 C53 1.50(2) . ?
C54 C55 1.51(2) . ?
C56 C58 1.49(3) . ?
C56 C57 1.50(3) . ?
