#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:35:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179337 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/34/4323484.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_4323484
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
;
(C10 H16 N +)3, (C12 Fe3 O12 Tl 3-)
;
_chemical_formula_structural
;
(((C7H7)N(CH3)3)3) (Tl(Fe(CO)4)3)
;
_chemical_formula_sum            'C42 H48 Fe3 N3 O12 Tl'
_chemical_formula_weight         1158.75
_chemical_name_systematic
; 
Tris Benzyltrimethyl ammonium thallium tris Iron Tetracarbonylate
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   18.290(3)
_cell_length_b                   18.290(3)
_cell_length_c                   8.479(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      8
_cell_measurement_theta_min      4
_cell_volume                     2456.4(8)
_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
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'RIGAKU AFC5S'
_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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1878
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.196
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       needle
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .2
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.009
_refine_ls_goodness_of_fit_obs   1.039
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         837
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.049
_refine_ls_restrained_S_obs      1.085
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_obs          0.0235
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0207P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0533
_refine_ls_wR_factor_obs         0.0494
_reflns_number_observed          708
_reflns_number_total             837
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961203k_4.cif
_cod_data_source_block           tlfe3cen
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0207P)^2^+0.0000P] 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^)+(0.0207P)^2^+0.0000P] 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               4323484
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Tl1 Tl 0.6667 0.3333 0.2500 0.0558(3) Uani 1 d S .
Fe1 Fe 0.49721(7) 0.26127(7) 0.2500 0.0574(4) Uani 1 d S .
C11 C 0.5179(4) 0.3214(4) 0.4247(10) 0.077(2) Uani 1 d . .
O11 O 0.5257(3) 0.3596(3) 0.5382(7) 0.112(2) Uani 1 d . .
C12 C 0.3895(7) 0.2147(6) 0.2500 0.087(3) Uani 1 d S .
O12 O 0.3160(5) 0.1829(4) 0.2500 0.146(4) Uani 1 d S .
C13 C 0.4954(5) 0.1656(6) 0.2500 0.064(3) Uani 1 d S .
O13 O 0.4897(4) 0.0980(4) 0.2500 0.090(2) Uani 1 d S .
N1 N 0.6716(5) 0.5849(5) 0.7566(29) 0.065(3) Uani 0.50 d PD -1
C10 C 0.6685(10) 0.6190(11) 0.5982(18) 0.102(5) Uani 0.50 d PD -1
H10A H 0.6545(10) 0.6627(11) 0.6102(18) 0.090(10) Uiso 0.50 calc PR -1
H10B H 0.6264(10) 0.5744(11) 0.5345(18) 0.090(10) Uiso 0.50 calc PR -1
H10C H 0.7226(10) 0.6417(11) 0.5480(18) 0.090(10) Uiso 0.50 calc PR -1
C9 C 0.6933(6) 0.5170(6) 0.7384(44) 0.099(6) Uani 0.50 d PD -1
H9A H 0.6523(6) 0.4733(6) 0.6719(44) 0.090(10) Uiso 0.50 calc PR -1
H9B H 0.6934(6) 0.4940(6) 0.8400(44) 0.090(10) Uiso 0.50 calc PR -1
H9C H 0.7482(6) 0.5401(6) 0.6915(44) 0.090(10) Uiso 0.50 calc PR -1
C8 C 0.5861(7) 0.5483(8) 0.8313(15) 0.092(5) Uani 0.50 d PD -1
H8A H 0.5716(7) 0.5917(8) 0.8438(15) 0.090(10) Uiso 0.50 calc PR -1
H8B H 0.5869(7) 0.5254(8) 0.9327(15) 0.090(10) Uiso 0.50 calc PR -1
H8C H 0.5449(7) 0.5043(8) 0.7652(15) 0.090(10) Uiso 0.50 calc PR -1
C7 C 0.7338(7) 0.6547(8) 0.8597(19) 0.086(5) Uani 0.50 d PD -1
H7A H 0.7460(7) 0.6325(8) 0.9538(19) 0.090(10) Uiso 0.50 calc PR -1
H7B H 0.7130(7) 0.6921(8) 0.8905(19) 0.090(10) Uiso 0.50 calc PR -1
C5 C 0.9241(10) 0.8312(10) 0.8381(22) 0.163(10) Uani 0.50 d PGDU -1
H5A H 0.9393(10) 0.8832(10) 0.8831(22) 0.090(10) Uiso 0.50 calc PR -1
C4 C 0.9827(9) 0.8073(10) 0.8204(20) 0.123(7) Uani 0.50 d PDU -1
H4A H 1.0352(9) 0.8373(10) 0.8689(20) 0.090(10) Uiso 0.50 calc PR -1
C3 C 0.9612(9) 0.7316(10) 0.7213(40) 0.088(8) Uani 0.50 d PDU -1
H3A H 1.0022(9) 0.7204(10) 0.6829(40) 0.090(10) Uiso 0.50 calc PR -1
C2 C 0.8805(8) 0.6822(9) 0.6921(16) 0.098(6) Uani 0.50 d PDU -1
H2A H 0.8620(8) 0.6313(9) 0.6395(16) 0.090(10) Uiso 0.50 calc PR -1
C1 C 0.8222(7) 0.7064(8) 0.7404(51) 0.158(10) Uani 0.50 d PDU -1
C6 C 0.8448(8) 0.7804(9) 0.7914(37) 0.104(13) Uani 0.50 d PDU -1
H5A H 0.8059(8) 0.7990(9) 0.7960(37) 0.090(10) Uiso 0.50 calc PR -1
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
Fe1 Tl1 Fe1 120.0 2_655 3_665 y
Fe1 Tl1 Fe1 120.0 2_655 . y
Fe1 Tl1 Fe1 120.0 3_665 . y
C12 Fe1 C13 93.5(4) . . ?
C12 Fe1 C11 98.3(3) . . ?
C13 Fe1 C11 121.2(2) . . ?
C12 Fe1 C11 98.3(3) . 10_556 ?
C13 Fe1 C11 121.2(2) . 10_556 ?
C11 Fe1 C11 113.7(4) . 10_556 ?
C12 Fe1 Tl1 179.5(3) . . ?
C13 Fe1 Tl1 86.0(3) . . ?
C11 Fe1 Tl1 81.9(2) . . ?
C11 Fe1 Tl1 81.9(2) 10_556 . ?
O11 C11 Fe1 175.2(7) . . ?
O12 C12 Fe1 180.0(12) . . ?
O13 C13 Fe1 176.6(7) . . ?
C9 N1 C7 111.5(11) . . ?
C9 N1 C10 109.6(16) . . ?
C7 N1 C10 110.0(10) . . ?
C9 N1 C8 108.9(10) . . ?
C7 N1 C8 108.2(13) . . ?
C10 N1 C8 108.5(11) . . ?
N1 C7 C1 103.2(14) . . ?
C6 C5 C4 120.3(15) . . ?
C5 C4 C3 118.6(14) . . ?
C2 C3 C4 115.4(16) . . ?
C3 C2 C1 119.8(15) . . ?
C6 C1 C2 122.6(12) . . ?
C6 C1 C7 95.7(23) . . ?
C2 C1 C7 130.3(13) . . ?
C1 C6 C5 120.0(13) . . ?
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 Fe1 2.6940(12) 2_655 y
Tl1 Fe1 2.6940(12) 3_665 y
Tl1 Fe1 2.6940(12) . y
Fe1 C12 1.711(11) . ?
Fe1 C13 1.734(10) . ?
Fe1 C11 1.769(9) . ?
Fe1 C11 1.769(9) 10_556 ?
C11 O11 1.155(8) . ?
C12 O12 1.168(10) . ?
C13 O13 1.188(9) . ?
N1 C9 1.489(10) . ?
N1 C7 1.495(15) . ?
N1 C10 1.49(2) . ?
N1 C8 1.499(13) . ?
C7 C1 1.73(3) . ?
C5 C6 1.33(2) . ?
C5 C4 1.35(2) . ?
C4 C3 1.49(3) . ?
C3 C2 1.31(2) . ?
C2 C1 1.40(2) . ?
C1 C6 1.28(2) . ?
