#------------------------------------------------------------------------------
#$Date: 2016-03-26 12:31:19 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180225 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/11/7111164.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_7111164
loop_
_publ_author_name
'Mosquera, Marta E. G.'
'Hopkins, Alexander D.'
'Raithby, Paul R.'
'Rothenberger, Alexander'
'Woods, Anthony D.'
'Wright, Dominic S.'
'Steiner, Alexander'
_publ_section_title
;
 Synthesis and structure of [{Sn4(NBut)3P}{Sn4(NBut)3(OSiMe3)}]; a
 low-oxidation state p-block metal complex containing a P3− anion
;
_journal_issue                   4
_journal_name_full               'Chemical Communications'
_journal_page_first              327
_journal_paper_doi               10.1039/b008108f
_journal_year                    2001
_chemical_formula_sum            'C27 H63 N6 O P Si Sn8'
_chemical_formula_weight         1496.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           8
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2y'
_symmetry_space_group_name_H-M   'C 1 m 1'
_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                 116.00(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.453(3)
_cell_length_b                   15.280(3)
_cell_length_c                   12.736(3)
_cell_measurement_reflns_used    15443
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2353.1(11)
_computing_molecular_graphics    'SHELXTL-PLUS (sheldrick, 1991)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    TeXsan
_diffrn_ambient_temperature      220(2)
_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  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10543
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    4.258
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   SORTAV
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.112
_exptl_crystal_description       Block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.799
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.153
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.53(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.056
_refine_ls_goodness_of_fit_obs   1.082
_refine_ls_hydrogen_treatment    'Riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         5238
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      2.227
_refine_ls_restrained_S_obs      1.082
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_obs          0.0425
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0245P)²+20.0967P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1928
_refine_ls_wR_factor_obs         0.0875
_reflns_number_observed          4605
_reflns_number_total             5252
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b008108fsup1.cif
_cod_data_source_block           dw9924
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+20.0967P] 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^)+(0.0245P)^2^+20.0967P] 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        2353.1(8)
_cod_original_sg_symbol_H-M      Cm
_cod_database_code               7111164
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, 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
Sn1 Sn 0.15462(7) 0.5000 0.32939(8) 0.0380(2) Uani 1 d S
Sn2 Sn 0.37491(7) 0.5000 0.58736(7) 0.0325(2) Uani 1 d S
Sn3 Sn 0.40484(5) 0.38835(5) 0.37749(6) 0.0424(2) Uani 1 d .
Sn4 Sn 0.21356(5) 0.38627(5) 0.03859(6) 0.0387(2) Uani 1 d .
Sn5 Sn 0.27741(7) 0.5000 -0.14413(7) 0.0314(2) Uani 1 d S
Sn6 Sn 0.47265(7) 0.5000 0.13417(7) 0.0357(2) Uani 1 d S
P1 P 0.2676(3) 0.5000 0.2100(3) 0.0452(9) Uani 1 d S
N1 N 0.4798(7) 0.5000 0.4955(9) 0.027(2) Uani 1 d S
C1 C 0.6071(11) 0.5000 0.5688(15) 0.051(4) Uani 1 d S
C11 C 0.6646(10) 0.5000 0.4863(15) 0.059(5) Uani 1 d S
H11A H 0.6459(10) 0.4467 0.4403(15) 0.088 Uiso 0.50 calc PR
H11B H 0.7442(10) 0.5031 0.5325(15) 0.088 Uiso 1 calc SR
H11C H 0.6398(10) 0.5502 0.4346(15) 0.088 Uiso 0.50 calc PR
C12 C 0.6323(10) 0.5831(9) 0.6460(12) 0.075(4) Uani 1 d .
H12A H 0.6163(10) 0.6348(9) 0.5970(12) 0.113 Uiso 1 calc R
H12B H 0.7098(10) 0.5833(9) 0.7017(12) 0.113 Uiso 1 calc R
H12C H 0.5868(10) 0.5833(9) 0.6876(12) 0.113 Uiso 1 calc R
N2 N 0.2794(6) 0.4059(5) 0.4466(6) 0.030(2) Uani 1 d .
C2 C 0.2369(8) 0.3254(7) 0.4766(8) 0.037(2) Uani 1 d .
C21 C 0.1635(9) 0.3478(8) 0.5375(10) 0.051(3) Uani 1 d .
H21A H 0.1022(9) 0.3841(8) 0.4863(10) 0.077 Uiso 1 calc R
H21B H 0.2068(9) 0.3791(8) 0.6094(10) 0.077 Uiso 1 calc R
H21C H 0.1350(9) 0.2942(8) 0.5550(10) 0.077 Uiso 1 calc R
C22 C 0.1646(12) 0.2746(8) 0.3578(10) 0.059(3) Uani 1 d .
H22A H 0.1033(12) 0.3113(8) 0.3076(10) 0.088 Uiso 1 calc R
H22B H 0.1363(12) 0.2209(8) 0.3751(10) 0.088 Uiso 1 calc R
H22C H 0.2103(12) 0.2609(8) 0.3186(10) 0.088 Uiso 1 calc R
C23 C 0.3325(10) 0.2688(7) 0.5553(10) 0.057(3) Uani 1 d .
H23A H 0.3784(10) 0.2550(7) 0.5163(10) 0.086 Uiso 1 calc R
H23B H 0.3044(10) 0.2151(7) 0.5729(10) 0.086 Uiso 1 calc R
H23C H 0.3762(10) 0.3000(7) 0.6273(10) 0.086 Uiso 1 calc R
N3 N 0.1499(9) 0.5000 -0.0781(10) 0.035(3) Uani 1 d S
C3 C 0.0321(10) 0.5000 -0.1654(12) 0.036(3) Uani 1 d S
C31 C -0.0424(13) 0.5000 -0.0993(16) 0.068(5) Uani 1 d S
H31A H -0.0246(13) 0.5505 -0.0480(16) 0.102 Uiso 0.50 calc PR
H31B H -0.0292(13) 0.4469 -0.0533(16) 0.102 Uiso 0.50 calc PR
H31C H -0.1196(13) 0.5026 -0.1555(16) 0.102 Uiso 1 calc SR
C32 C 0.0012(9) 0.4213(8) -0.2424(11) 0.066(4) Uani 1 d .
H32A H 0.0203(9) 0.3688(8) -0.1947(11) 0.099 Uiso 1 calc R
H32B H 0.0408(9) 0.4219(8) -0.2902(11) 0.099 Uiso 1 calc R
H32C H -0.0778(9) 0.4219(8) -0.2924(11) 0.099 Uiso 1 calc R
N4 N 0.3539(5) 0.4064(5) -0.0007(6) 0.026(2) Uani 1 d .
C4 C 0.3996(8) 0.3217(7) -0.0263(8) 0.037(2) Uani 1 d .
C41 C 0.3051(10) 0.2616(9) -0.1131(10) 0.055(3) Uani 1 d .
H41A H 0.2640(10) 0.2927(9) -0.1859(10) 0.083 Uiso 1 calc R
H41B H 0.2556(10) 0.2459(9) -0.0791(10) 0.083 Uiso 1 calc R
H41C H 0.3370(10) 0.2089(9) -0.1282(10) 0.083 Uiso 1 calc R
C42 C 0.4652(10) 0.2750(7) 0.0883(11) 0.051(3) Uani 1 d .
H42A H 0.4171(10) 0.2613(7) 0.1248(11) 0.077 Uiso 1 calc R
H42B H 0.5250(10) 0.3124(7) 0.1397(11) 0.077 Uiso 1 calc R
H42C H 0.4957(10) 0.2213(7) 0.0739(11) 0.077 Uiso 1 calc R
C43 C 0.4759(10) 0.3439(8) -0.0854(9) 0.054(3) Uani 1 d .
H43A H 0.4334(10) 0.3738(8) -0.1588(9) 0.081 Uiso 1 calc R
H43B H 0.5064(10) 0.2903(8) -0.1001(9) 0.081 Uiso 1 calc R
H43C H 0.5357(10) 0.3815(8) -0.0343(9) 0.081 Uiso 1 calc R
Si1 Si 0.7300(4) 0.5000 0.1435(4) 0.0544(11) Uani 1 d S
O1 O 0.5945(8) 0.5000 0.0868(10) 0.057(3) Uani 1 d S
C51 C 0.7718(22) 0.5000 0.0315(28) 0.149(12) Uani 1 d S
H51A H 0.7418(22) 0.4489 -0.0175(28) 0.223 Uiso 0.50 calc PR
H51B H 0.8519(22) 0.4985 0.0651(28) 0.223 Uiso 1 calc SR
H51C H 0.7449(22) 0.5526 -0.0152(28) 0.223 Uiso 0.50 calc PR
C52 C 0.7891(19) 0.5990(12) 0.2361(24) 0.172(13) Uani 1 d .
H52A H 0.7667(19) 0.6000(12) 0.2989(24) 0.258 Uiso 1 calc R
H52B H 0.7622(19) 0.6512(12) 0.1887(24) 0.258 Uiso 1 calc R
H52C H 0.8692(19) 0.5971(12) 0.2689(24) 0.258 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'
Si Si 0.0817 0.0704 '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'
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
N2 Sn1 N2 80.9(4) 2_565 .
N2 Sn1 P1 85.9(2) 2_565 .
N2 Sn1 P1 85.9(2) . .
N1 Sn2 N2 81.3(3) . .
N1 Sn2 N2 81.3(3) . 2_565
N2 Sn2 N2 80.9(4) . 2_565
N1 Sn3 N2 80.6(3) . .
N1 Sn3 P1 90.0(2) . .
N2 Sn3 P1 82.2(2) . .
N4 Sn4 N3 81.6(3) . .
N4 Sn4 P1 98.3(2) . .
N3 Sn4 P1 85.6(3) . .
N4 Sn5 N4 81.6(4) 2_565 .
N4 Sn5 N3 80.9(3) 2_565 .
N4 Sn5 N3 80.9(3) . .
O1 Sn6 N4 99.9(3) . .
O1 Sn6 N4 99.9(3) . 2_565
N4 Sn6 N4 78.2(3) . 2_565
Sn1 P1 Sn4 117.99(11) . .
Sn1 P1 Sn4 117.99(11) . 2_565
Sn4 P1 Sn4 82.67(11) . 2_565
Sn1 P1 Sn3 84.87(10) . 2_565
Sn4 P1 Sn3 155.4(2) . 2_565
Sn4 P1 Sn3 94.70(5) 2_565 2_565
Sn1 P1 Sn3 84.87(10) . .
Sn4 P1 Sn3 94.70(5) . .
Sn4 P1 Sn3 155.4(2) 2_565 .
Sn3 P1 Sn3 77.58(11) 2_565 .
C1 N1 Sn2 118.6(8) . .
C1 N1 Sn3 117.7(4) . .
Sn2 N1 Sn3 98.9(3) . .
C1 N1 Sn3 117.7(4) . 2_565
Sn2 N1 Sn3 98.9(3) . 2_565
Sn3 N1 Sn3 101.5(4) . 2_565
C12 C1 C12 110.0(15) . 2_565
C12 C1 N1 105.0(8) . .
C12 C1 N1 105.0(8) 2_565 .
C12 C1 C11 113.2(8) . .
C12 C1 C11 113.2(8) 2_565 .
N1 C1 C11 109.8(12) . .
C2 N2 Sn2 119.0(5) . .
C2 N2 Sn1 116.7(6) . .
Sn2 N2 Sn1 97.1(3) . .
C2 N2 Sn3 116.6(6) . .
Sn2 N2 Sn3 97.3(3) . .
Sn1 N2 Sn3 107.0(3) . .
N2 C2 C23 109.6(8) . .
N2 C2 C21 110.7(8) . .
C23 C2 C21 110.0(8) . .
N2 C2 C22 107.7(7) . .
C23 C2 C22 109.8(10) . .
C21 C2 C22 109.1(8) . .
C3 N3 Sn4 118.5(4) . 2_565
C3 N3 Sn4 118.5(4) . .
Sn4 N3 Sn4 104.3(5) 2_565 .
C3 N3 Sn5 117.7(8) . .
Sn4 N3 Sn5 96.8(3) 2_565 .
Sn4 N3 Sn5 96.8(3) . .
N3 C3 C32 113.0(7) . .
N3 C3 C32 113.0(7) . 2_565
C32 C3 C32 107.5(13) . 2_565
N3 C3 C31 108.8(11) . .
C32 C3 C31 107.1(8) . .
C32 C3 C31 107.1(8) 2_565 .
C4 N4 Sn4 113.5(6) . .
C4 N4 Sn5 117.5(5) . .
Sn4 N4 Sn5 98.4(3) . .
C4 N4 Sn6 118.7(5) . .
Sn4 N4 Sn6 108.0(3) . .
Sn5 N4 Sn6 97.9(3) . .
C42 C4 N4 108.3(7) . .
C42 C4 C43 109.9(9) . .
N4 C4 C43 109.3(8) . .
C42 C4 C41 110.8(10) . .
N4 C4 C41 111.7(8) . .
C43 C4 C41 106.9(8) . .
O1 Si1 C51 109.5(10) . .
O1 Si1 C52 111.2(8) . .
C51 Si1 C52 108.4(10) . .
O1 Si1 C52 111.2(8) . 2_565
C51 Si1 C52 108.4(10) . 2_565
C52 Si1 C52 108.1(17) . 2_565
Si1 O1 Sn6 140.8(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 N2 2.218(8) 2_565
Sn1 N2 2.218(7) .
Sn1 P1 2.579(4) .
Sn2 N1 2.192(10) .
Sn2 N2 2.217(8) .
Sn2 N2 2.217(8) 2_565
Sn3 N1 2.204(6) .
Sn3 N2 2.235(7) .
Sn3 P1 2.723(3) .
Sn4 N4 2.177(7) .
Sn4 N3 2.201(7) .
Sn4 P1 2.631(3) .
Sn5 N4 2.189(7) 2_565
Sn5 N4 2.189(7) .
Sn5 N3 2.217(11) .
Sn6 O1 1.980(9) .
Sn6 N4 2.267(8) .
Sn6 N4 2.267(8) 2_565
P1 Sn4 2.631(3) 2_565
P1 Sn3 2.723(3) 2_565
N1 C1 1.55(2) .
N1 Sn3 2.204(6) 2_565
C1 C12 1.55(2) .
C1 C12 1.55(2) 2_565
C1 C11 1.55(2) .
N2 C2 1.476(12) .
C2 C23 1.509(15) .
C2 C21 1.537(14) .
C2 C22 1.595(13) .
N3 C3 1.48(2) .
N3 Sn4 2.201(7) 2_565
C3 C32 1.492(14) .
C3 C32 1.492(14) 2_565
C3 C31 1.57(2) .
N4 C4 1.528(11) .
C4 C42 1.513(14) .
C4 C43 1.554(14) .
C4 C41 1.565(15) .
Si1 O1 1.640(11) .
Si1 C51 1.75(3) .
Si1 C52 1.87(2) .
Si1 C52 1.87(2) 2_565
