#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:30:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179331 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/28/4322802.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_4322802
loop_
_publ_author_name
'Robert E. Allan'
'Michael A. Beswick'
'Neil Feeder'
'Michael Kranz'
'Marta E. G. Mosquera'
'Paul R. Raithby'
'Andrew E. H. Wheatley'
'Dominic S. Wright'
_publ_section_title
;
 Synthesis and Structure of the Heterobimetallic Ladder Complex
 [{(MesNH)Sn(μ-Nma)}2(Li.2THF)2] (Mes = 2,4,6-Me3C6H2, ma = 2-MeOC6H4)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2602
_journal_page_last               2604
_journal_paper_doi               10.1021/ic971093x
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C48 H70 Li2 N4 O6 Sn2'
_chemical_formula_weight         1050.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                104.45(4)
_cell_angle_beta                 99.70(5)
_cell_angle_gamma                102.01(5)
_cell_formula_units_Z            1
_cell_length_a                   11.080(7)
_cell_length_b                   11.720(7)
_cell_length_c                   10.561(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_volume                     1263.3(14)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       AFC5R
_diffrn_measurement_method       'omega/2theta scans'
_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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0862
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6091
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        0.4%
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.036
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.961
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.078
_refine_ls_goodness_of_fit_obs   1.100
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         5794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_restrained_S_obs      1.100
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_obs          0.0463
_refine_ls_shift/esd_max         -0.135
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0567P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1287
_refine_ls_wR_factor_obs         0.1143
_reflns_number_observed          4454
_reflns_number_total             5795
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971093x.cif
_cod_data_source_block           dw970
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0567P)^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^)+(0.0567P)^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_original_cell_volume        1263.3(13)
_cod_database_code               4322802
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
Li1 Li 0.6764(8) 0.3864(8) -0.0922(9) 0.036(2) Uani 1 d . .
Sn1 Sn 0.52448(3) 0.48200(3) 0.15423(3) 0.02504(10) Uani 1 d . .
O1 O 0.4821(4) 0.2367(3) 0.1144(4) 0.0381(8) Uani 1 d . .
O2 O 0.6987(4) 0.2457(4) -0.2233(4) 0.0489(10) Uani 1 d . .
O3 O 0.8080(4) 0.3952(4) 0.0660(4) 0.0462(10) Uani 1 d . .
N1 N 0.4966(4) 0.3789(3) -0.0529(4) 0.0264(8) Uani 1 d . .
N2 N 0.3127(4) 0.4473(4) 0.1308(4) 0.0285(8) Uani 1 d . .
H2N H 0.2802(51) 0.4012(48) 0.0450(55) 0.034 Uiso 1 d . .
C1 C 0.4559(6) 0.1768(5) 0.2130(6) 0.0472(14) Uani 1 d . .
H1A H 0.4949(35) 0.2334(13) 0.3031(6) 0.071 Uiso 1 calc R .
H1B H 0.4908(36) 0.1056(23) 0.2009(28) 0.071 Uiso 1 calc R .
H1C H 0.3639(6) 0.1502(35) 0.2025(28) 0.071 Uiso 1 calc R .
C2 C 0.4177(5) 0.1797(4) -0.0179(5) 0.0337(11) Uani 1 d . .
C3 C 0.3509(5) 0.0579(5) -0.0652(6) 0.0444(13) Uani 1 d . .
H3A H 0.3507(5) 0.0082(5) -0.0066(6) 0.053 Uiso 1 calc R .
C4 C 0.2846(7) 0.0087(5) -0.1977(7) 0.060(2) Uani 1 d . .
H4A H 0.2385(7) -0.0748(5) -0.2304(7) 0.072 Uiso 1 calc R .
C5 C 0.2855(7) 0.0811(5) -0.2822(6) 0.058(2) Uani 1 d . .
H5A H 0.2373(7) 0.0479(5) -0.3725(6) 0.069 Uiso 1 calc R .
C6 C 0.3566(6) 0.2032(5) -0.2365(6) 0.0478(15) Uani 1 d . .
H6A H 0.3581(6) 0.2503(5) -0.2978(6) 0.057 Uiso 1 calc R .
C7 C 0.4261(5) 0.2584(4) -0.1023(5) 0.0299(10) Uani 1 d . .
C8 C 0.2525(4) 0.3844(4) 0.2092(5) 0.0263(9) Uani 1 d . .
C9 C 0.2850(4) 0.4334(5) 0.3516(5) 0.0305(10) Uani 1 d . .
C10 C 0.2293(5) 0.3677(5) 0.4293(5) 0.0379(12) Uani 1 d . .
H10A H 0.2538(5) 0.4008(5) 0.5244(5) 0.046 Uiso 1 calc R .
C11 C 0.1393(5) 0.2558(5) 0.3740(6) 0.0393(12) Uani 1 d . .
C12 C 0.1043(5) 0.2112(5) 0.2348(6) 0.0366(12) Uani 1 d . .
H12A H 0.0414(5) 0.1359(5) 0.1945(6) 0.044 Uiso 1 calc R .
C13 C 0.1572(4) 0.2722(4) 0.1512(5) 0.0299(10) Uani 1 d . .
C14 C 0.3756(5) 0.5580(5) 0.4195(5) 0.0424(13) Uani 1 d . .
H14A H 0.3635(27) 0.5894(17) 0.5103(16) 0.064 Uiso 1 calc R .
H14B H 0.3591(26) 0.6137(11) 0.3672(22) 0.064 Uiso 1 calc R .
H14C H 0.4631(5) 0.5517(8) 0.4251(37) 0.064 Uiso 1 calc R .
C15 C 0.0783(6) 0.1879(7) 0.4617(7) 0.059(2) Uani 1 d . .
H15A H 0.0638(42) 0.0999(7) 0.4215(26) 0.088 Uiso 1 calc R .
H15B H -0.0029(22) 0.2068(35) 0.4687(40) 0.088 Uiso 1 calc R .
H15C H 0.1346(21) 0.2133(33) 0.5515(16) 0.088 Uiso 1 calc R .
C16 C 0.1090(5) 0.2214(5) 0.0007(5) 0.0416(13) Uani 1 d . .
H16A H 0.0430(27) 0.1448(19) -0.0210(6) 0.062 Uiso 1 calc R .
H16B H 0.1792(9) 0.2059(34) -0.0405(6) 0.062 Uiso 1 calc R .
H16C H 0.0735(34) 0.2804(16) -0.0342(7) 0.062 Uiso 1 calc R .
C17 C 0.6390(11) 0.1214(7) -0.2695(13) 0.122(5) Uani 1 d . .
H17A H 0.6267(11) 0.0912(7) -0.1918(13) 0.146 Uiso 1 calc R .
H17B H 0.5542(11) 0.1084(7) -0.3275(13) 0.146 Uiso 1 calc R .
C18 C 0.7050(15) 0.0572(8) -0.3388(17) 0.202(9) Uani 1 d . .
H18A H 0.6511(15) 0.0060(8) -0.4278(17) 0.243 Uiso 1 calc R .
H18B H 0.7359(15) 0.0033(8) -0.2897(17) 0.243 Uiso 1 calc R .
C19 C 0.8111(15) 0.1439(10) -0.3549(15) 0.190(9) Uani 1 d . .
H19A H 0.8908(15) 0.1196(10) -0.3337(15) 0.228 Uiso 1 calc R .
H19B H 0.7971(15) 0.1489(10) -0.4482(15) 0.228 Uiso 1 calc R .
C20 C 0.8171(7) 0.2593(7) -0.2615(9) 0.077(2) Uani 1 d . .
H20A H 0.8878(7) 0.2797(7) -0.1818(9) 0.092 Uiso 1 calc R .
H20B H 0.8304(7) 0.3254(7) -0.3047(9) 0.092 Uiso 1 calc R .
C21 C 0.8978(7) 0.5014(7) 0.1607(7) 0.070(2) Uani 1 d . .
H21A H 0.8581(7) 0.5703(7) 0.1794(7) 0.083 Uiso 1 calc R .
H21B H 0.9721(7) 0.5260(7) 0.1237(7) 0.083 Uiso 1 calc R .
C22 C 0.9383(6) 0.4697(6) 0.2871(6) 0.0493(14) Uani 1 d . .
H22A H 0.9413(6) 0.5365(6) 0.3673(6) 0.059 Uiso 1 calc R .
H22B H 1.0228(6) 0.4531(6) 0.2936(6) 0.059 Uiso 1 calc R .
C23 C 0.8363(6) 0.3554(6) 0.2737(6) 0.0477(14) Uani 1 d . .
H23A H 0.8706(6) 0.3018(6) 0.3210(6) 0.057 Uiso 1 calc R .
H23B H 0.7638(6) 0.3761(6) 0.3091(6) 0.057 Uiso 1 calc R .
C24 C 0.7985(5) 0.2968(5) 0.1247(6) 0.0445(14) Uani 1 d . .
H24A H 0.8559(5) 0.2463(5) 0.0958(6) 0.053 Uiso 1 calc R .
H24B H 0.7105(5) 0.2442(5) 0.0975(6) 0.053 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'
Li Li -0.0003 0.0001 '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'
Sn Sn -0.6537 1.4246 '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'
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
O2 Li1 O3 99.4(4) . . ?
O2 Li1 N2 121.6(5) . 2_665 ?
O3 Li1 N2 113.3(5) . 2_665 ?
O2 Li1 N1 118.3(5) . . ?
O3 Li1 N1 113.6(5) . . ?
N2 Li1 N1 91.7(4) 2_665 . ?
O2 Li1 Sn1 123.2(4) . 2_665 ?
O3 Li1 Sn1 137.4(4) . 2_665 ?
N2 Li1 Sn1 48.0(2) 2_665 2_665 ?
N1 Li1 Sn1 46.2(2) . 2_665 ?
O2 Li1 Sn1 145.9(4) . . ?
O3 Li1 Sn1 81.5(3) . . ?
N2 Li1 Sn1 88.0(3) 2_665 . ?
N1 Li1 Sn1 37.1(2) . . ?
Sn1 Li1 Sn1 62.4(2) 2_665 . ?
N1 Sn1 N1 78.8(2) . 2_665 ?
N1 Sn1 N2 90.4(2) . . ?
N1 Sn1 N2 84.36(15) 2_665 . ?
N1 Sn1 Li1 93.6(2) . 2_665 ?
N1 Sn1 Li1 43.6(2) 2_665 2_665 ?
N2 Sn1 Li1 43.1(2) . 2_665 ?
N1 Sn1 Li1 35.8(2) . . ?
N1 Sn1 Li1 83.1(2) 2_665 . ?
N2 Sn1 Li1 126.1(2) . . ?
Li1 Sn1 Li1 117.6(2) 2_665 . ?
C2 O1 C1 118.4(4) . . ?
C17 O2 C20 106.1(5) . . ?
C17 O2 Li1 134.9(5) . . ?
C20 O2 Li1 117.1(5) . . ?
C24 O3 C21 108.3(4) . . ?
C24 O3 Li1 120.7(4) . . ?
C21 O3 Li1 128.5(4) . . ?
C7 N1 Li1 107.7(4) . . ?
C7 N1 Sn1 121.5(3) . . ?
Li1 N1 Sn1 107.1(3) . . ?
C7 N1 Sn1 123.9(3) . 2_665 ?
Li1 N1 Sn1 90.2(3) . 2_665 ?
Sn1 N1 Sn1 101.2(2) . 2_665 ?
C8 N2 Li1 136.6(4) . 2_665 ?
C8 N2 Sn1 120.0(3) . . ?
Li1 N2 Sn1 88.9(3) 2_665 . ?
O1 C2 C3 123.3(5) . . ?
O1 C2 C7 113.9(4) . . ?
C3 C2 C7 122.9(5) . . ?
C4 C3 C2 119.9(5) . . ?
C5 C4 C3 119.8(5) . . ?
C4 C5 C6 120.7(6) . . ?
C5 C6 C7 122.0(5) . . ?
N1 C7 C6 123.8(5) . . ?
N1 C7 C2 121.5(4) . . ?
C6 C7 C2 114.7(5) . . ?
N2 C8 C13 122.1(4) . . ?
N2 C8 C9 119.9(4) . . ?
C13 C8 C9 118.0(4) . . ?
C10 C9 C8 119.7(5) . . ?
C10 C9 C14 119.4(5) . . ?
C8 C9 C14 120.9(4) . . ?
C11 C10 C9 122.9(5) . . ?
C12 C11 C10 117.0(5) . . ?
C12 C11 C15 121.5(5) . . ?
C10 C11 C15 121.5(5) . . ?
C11 C12 C13 122.9(5) . . ?
C12 C13 C8 119.5(5) . . ?
C12 C13 C16 119.8(5) . . ?
C8 C13 C16 120.7(4) . . ?
C18 C17 O2 112.5(8) . . ?
C17 C18 C19 107.2(8) . . ?
C20 C19 C18 105.3(8) . . ?
O2 C20 C19 106.5(7) . . ?
O3 C21 C22 107.8(5) . . ?
C21 C22 C23 103.7(5) . . ?
C24 C23 C22 102.1(5) . . ?
O3 C24 C23 105.8(5) . . ?
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
Li1 O2 1.960(10) . ?
Li1 O3 1.990(10) . ?
Li1 N2 2.072(10) 2_665 ?
Li1 N1 2.091(10) . ?
Li1 Sn1 3.034(9) 2_665 ?
Li1 Sn1 3.415(9) . ?
Sn1 N1 2.154(4) . ?
Sn1 N1 2.191(4) 2_665 ?
Sn1 N2 2.257(4) . ?
Sn1 Li1 3.034(9) 2_665 ?
O1 C2 1.382(6) . ?
O1 C1 1.430(6) . ?
O2 C17 1.391(8) . ?
O2 C20 1.425(8) . ?
O3 C24 1.433(6) . ?
O3 C21 1.437(7) . ?
N1 C7 1.383(6) . ?
N1 Sn1 2.191(4) 2_665 ?
N2 C8 1.401(6) . ?
N2 Li1 2.072(10) 2_665 ?
C2 C3 1.384(7) . ?
C2 C7 1.433(7) . ?
C3 C4 1.380(9) . ?
C4 C5 1.376(9) . ?
C5 C6 1.400(8) . ?
C6 C7 1.410(7) . ?
C8 C13 1.421(7) . ?
C8 C9 1.421(7) . ?
C9 C10 1.391(7) . ?
C9 C14 1.510(7) . ?
C10 C11 1.390(8) . ?
C11 C12 1.388(8) . ?
C11 C15 1.517(7) . ?
C12 C13 1.396(7) . ?
C13 C16 1.509(7) . ?
C17 C18 1.331(12) . ?
C18 C19 1.448(13) . ?
C19 C20 1.444(11) . ?
C21 C22 1.495(8) . ?
C22 C23 1.521(8) . ?
C23 C24 1.497(8) . ?
