#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:46:24 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179814 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/10/7011023.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_7011023
loop_
_publ_author_name
'Claudio Pettinari'
'Fabio Marchetti'
'Riccardo Pettinari'
'Augusto Cingolani'
'Andrei Drozdov'
'Sergei Troyanov'
_publ_section_title
;
 The interaction of organotin(IV) acceptors with
 1,4-bis(5-hydroxy-1-phenyl-3-methyl-1H-pyrazol-4-yl)butane-1,4-dione
;
_journal_issue                   2
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              188
_journal_page_last               194
_journal_paper_doi               10.1039/b106665j
_journal_year                    2002
_chemical_formula_sum            'C64 H76 N8 O8 Sn2'
_chemical_formula_weight         1322.71
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 127.39(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.419(5)
_cell_length_b                   18.696(3)
_cell_length_c                   16.978(4)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      24.8
_cell_measurement_theta_min      3.3
_cell_volume                     5906(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measurement_device       IPDS(Stoe)
_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  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25489
_diffrn_reflns_theta_max         27.06
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    0.909
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.031
_refine_ls_goodness_of_fit_obs   1.091
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         5452
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_restrained_S_obs      1.091
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_obs          0.0250
_refine_ls_shift/esd_max         -0.009
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0325P)²+3.8629P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0679
_refine_ls_wR_factor_obs         0.0609
_reflns_number_observed          4698
_reflns_number_total             6424
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b106665j.txt
_cod_data_source_block           Q2QSn(Bu)2
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+3.8629P] 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^)+(0.0325P)^2^+3.8629P] 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        5906.2(21)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7011023
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Sn1 Sn 0.5000 0.279071(10) 0.2500 0.02638(7) Uani 1 d S 1
Sn2 Sn 0.5000 -0.092051(11) 0.2500 0.03129(7) Uani 1 d S 1
O1 O 0.39157(8) 0.25521(8) 0.19014(12) 0.0326(4) Uani 1 d . 1
O2 O 0.48507(9) 0.18709(9) 0.15747(13) 0.0385(4) Uani 1 d . 1
O3 O 0.49706(8) 0.00197(8) 0.16923(12) 0.0323(3) Uani 1 d . 1
O4 O 0.61267(9) -0.07290(9) 0.34138(13) 0.0346(4) Uani 1 d . 1
N1 N 0.28536(10) 0.19148(10) 0.10106(13) 0.0289(4) Uani 1 d . 1
N2 N 0.25355(10) 0.13415(10) 0.03498(14) 0.0330(4) Uani 1 d . 1
N3 N 0.71625(10) -0.04432(10) 0.35964(14) 0.0312(4) Uani 1 d . 1
N4 N 0.73804(10) -0.00262(10) 0.31390(15) 0.0331(4) Uani 1 d . 1
C1 C 0.35283(11) 0.20468(11) 0.1306(2) 0.0267(4) Uani 1 d . 1
C2 C 0.36599(12) 0.15358(11) 0.0813(2) 0.0275(4) Uani 1 d . 1
C3 C 0.30107(12) 0.11243(12) 0.0231(2) 0.0305(5) Uani 1 d . 1
C4 C 0.28192(14) 0.05094(13) -0.0447(2) 0.0378(5) Uani 1 d . 1
H4A H 0.3138(6) 0.0117(3) -0.0076(3) 0.057 Uiso 1 calc R 1
H4B H 0.2864(9) 0.0650(3) -0.0951(8) 0.057 Uiso 1 calc R 1
H4C H 0.2333(3) 0.0365(6) -0.0751(10) 0.057 Uiso 1 calc R 1
C5 C 0.24814(12) 0.22226(12) 0.1349(2) 0.0291(5) Uani 1 d . 1
C6 C 0.26632(13) 0.28939(13) 0.1781(2) 0.0368(5) Uani 1 d . 1
H6 H 0.30178(13) 0.31613(13) 0.1828(2) 0.044 Uiso 1 calc R 1
C7 C 0.23118(14) 0.31641(15) 0.2142(2) 0.0421(6) Uani 1 d . 1
H7 H 0.24379(14) 0.36123(15) 0.2441(2) 0.051 Uiso 1 calc R 1
C8 C 0.17808(14) 0.27801(14) 0.2065(2) 0.0438(6) Uani 1 d . 1
H8 H 0.15501(14) 0.29659(14) 0.2313(2) 0.053 Uiso 1 calc R 1
C9 C 0.15930(15) 0.2121(2) 0.1622(2) 0.0518(7) Uani 1 d . 1
H9 H 0.12304(15) 0.1861(2) 0.1564(2) 0.062 Uiso 1 calc R 1
C10 C 0.19388(13) 0.18369(14) 0.1257(2) 0.0421(6) Uani 1 d . 1
H10 H 0.18069(13) 0.13903(14) 0.0954(2) 0.051 Uiso 1 calc R 1
C11 C 0.43136(12) 0.14968(11) 0.0946(2) 0.0286(5) Uani 1 d . 1
C12 C 0.44156(13) 0.10281(11) 0.0316(2) 0.0309(5) Uani 1 d . 1
H12A H 0.42434(13) 0.12806(11) -0.0290(2) 0.037 Uiso 1 calc R 1
H12B H 0.41284(13) 0.05985(11) 0.0135(2) 0.037 Uiso 1 calc R 1
C13 C 0.51949(12) 0.08178(11) 0.0842(2) 0.0293(5) Uani 1 d . 1
H13A H 0.52488(12) 0.06215(11) 0.0361(2) 0.035 Uiso 1 calc R 1
H13B H 0.54939(12) 0.12416(11) 0.1127(2) 0.035 Uiso 1 calc R 1
C14 C 0.54497(12) 0.02771(11) 0.1646(2) 0.0268(4) Uani 1 d . 1
C15 C 0.64430(12) -0.03996(11) 0.3113(2) 0.0285(5) Uani 1 d . 1
C16 C 0.61733(12) 0.00650(11) 0.2299(2) 0.0273(4) Uani 1 d . 1
C17 C 0.67972(12) 0.02702(11) 0.2378(2) 0.0292(5) Uani 1 d . 1
C18 C 0.68590(14) 0.07566(13) 0.1737(2) 0.0374(5) Uani 1 d . 1
H18A H 0.6743(9) 0.1236(2) 0.1797(10) 0.056 Uiso 1 calc R 1
H18B H 0.6532(7) 0.0604(6) 0.1059(3) 0.056 Uiso 1 calc R 1
H18C H 0.7342(3) 0.0743(7) 0.1942(9) 0.056 Uiso 1 calc R 1
C19 C 0.76970(13) -0.07653(12) 0.4524(2) 0.0336(5) Uani 1 d . 1
C20 C 0.83884(14) -0.04967(14) 0.5079(2) 0.0435(6) Uani 1 d . 1
H20 H 0.85029(14) -0.01245(14) 0.4834(2) 0.052 Uiso 1 calc R 1
C21 C 0.8906(2) -0.0784(2) 0.5997(2) 0.0538(7) Uani 1 d . 1
H21 H 0.9373(2) -0.0609(2) 0.6368(2) 0.065 Uiso 1 calc R 1
C22 C 0.8738(2) -0.1331(2) 0.6371(2) 0.0562(8) Uani 1 d . 1
H22 H 0.9088(2) -0.1517(2) 0.6997(2) 0.067 Uiso 1 calc R 1
C23 C 0.8051(2) -0.1597(2) 0.5811(2) 0.0515(7) Uani 1 d . 1
H23 H 0.7938(2) -0.1967(2) 0.6062(2) 0.062 Uiso 1 calc R 1
C24 C 0.75261(15) -0.13244(13) 0.4883(2) 0.0413(6) Uani 1 d . 1
H24 H 0.70637(15) -0.15131(13) 0.4503(2) 0.050 Uiso 1 calc R 1
C25 C 0.48586(14) 0.34703(14) 0.1377(2) 0.0412(6) Uani 1 d . 1
H25A H 0.48838(14) 0.31856(14) 0.0921(2) 0.049 Uiso 1 calc R 1
H25B H 0.43875(14) 0.36915(14) 0.1004(2) 0.049 Uiso 1 calc R 1
C26 C 0.5452(2) 0.40677(15) 0.1848(2) 0.0500(7) Uani 1 d . 1
H26A H 0.5425(2) 0.43452(15) 0.2307(2) 0.060 Uiso 1 calc R 1
H26B H 0.5920(2) 0.38400(15) 0.2227(2) 0.060 Uiso 1 calc R 1
C27 C 0.5394(2) 0.4563(2) 0.1117(2) 0.0582(8) Uani 1 d . 1
H27A H 0.4930(2) 0.4798(2) 0.0743(2) 0.070 Uiso 1 calc R 1
H27B H 0.5420(2) 0.4289(2) 0.0655(2) 0.070 Uiso 1 calc R 1
C28 C 0.5975(2) 0.5119(2) 0.1602(3) 0.0708(9) Uani 1 d . 1
H28A H 0.5923(8) 0.5418(9) 0.1102(3) 0.106 Uiso 1 calc R 1
H28B H 0.6436(2) 0.4889(2) 0.1976(16) 0.106 Uiso 1 calc R 1
H28C H 0.5937(9) 0.5406(9) 0.2037(15) 0.106 Uiso 1 calc R 1
C29 C 0.5049(2) -0.1555(2) 0.3583(3) 0.0725(11) Uani 0.575(7) d P 1
H29A H 0.5440(2) -0.1362(2) 0.4224(3) 0.087 Uiso 1 calc R 1
H29B H 0.4611(2) -0.1458(2) 0.3506(3) 0.087 Uiso 1 calc R 1
C30 C 0.5137(3) -0.2308(2) 0.3660(3) 0.0361(13) Uani 0.575(7) d P 1
H30A H 0.5483(3) -0.2433(2) 0.3547(3) 0.043 Uiso 0.575(7) calc PR 1
H30B H 0.4682(3) -0.2524(2) 0.3134(3) 0.043 Uiso 0.575(7) calc PR 1
C31 C 0.5380(2) -0.2633(2) 0.4630(3) 0.0738(11) Uani 0.575(7) d P 1
H31A H 0.5128(2) -0.2368(2) 0.4824(3) 0.089 Uiso 1 calc R 1
H31B H 0.5175(2) -0.3110(2) 0.4463(3) 0.089 Uiso 1 calc R 1
C32 C 0.6115(2) -0.2722(2) 0.5548(3) 0.0756(10) Uani 1 d . 1
H32A H 0.6109(3) -0.3040(12) 0.5986(9) 0.113 Uiso 1 calc R 1
H32B H 0.6300(6) -0.2265(3) 0.5863(11) 0.113 Uiso 1 calc R 1
H32C H 0.6415(4) -0.2918(14) 0.5393(4) 0.113 Uiso 1 calc R 1
C29A C 0.5049(2) -0.1555(2) 0.3583(3) 0.0725(11) Uani 0.425(7) d P 2
C30A C 0.5614(3) -0.1957(3) 0.4211(4) 0.035(2) Uani 0.425(7) d P 2
H30C H 0.5986(3) -0.1669(3) 0.4766(4) 0.042 Uiso 0.425(7) calc PR 2
H30D H 0.5804(3) -0.2153(3) 0.3884(4) 0.042 Uiso 0.425(7) calc PR 2
C31A C 0.5380(2) -0.2633(2) 0.4630(3) 0.0738(11) Uani 0.425(7) d P 2
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'
Sn Sn -0.6537 1.4246 '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
O1 Sn1 O1 155.84(8) . 2_655 ?
O1 Sn1 C25 92.52(8) . 2_655 ?
O1 Sn1 C25 101.78(9) 2_655 2_655 ?
O1 Sn1 C25 101.78(9) . . ?
O1 Sn1 C25 92.52(8) 2_655 . ?
C25 Sn1 C25 107.28(14) 2_655 . ?
O1 Sn1 O2 82.52(6) . . ?
O1 Sn1 O2 78.72(6) 2_655 . ?
C25 Sn1 O2 165.11(8) 2_655 . ?
C25 Sn1 O2 87.51(8) . . ?
O1 Sn1 O2 78.72(6) . 2_655 ?
O1 Sn1 O2 82.52(6) 2_655 2_655 ?
C25 Sn1 O2 87.51(8) 2_655 2_655 ?
C25 Sn1 O2 165.11(8) . 2_655 ?
O2 Sn1 O2 77.77(10) . 2_655 ?
O4 Sn2 O4 160.62(9) 2_655 . ?
O4 Sn2 C29 96.67(11) 2_655 . ?
O4 Sn2 C29 94.07(12) . . ?
O4 Sn2 C29 94.07(12) 2_655 2_655 ?
O4 Sn2 C29 96.67(11) . 2_655 ?
C29 Sn2 C29 112.4(2) . 2_655 ?
O4 Sn2 O3 82.87(6) 2_655 2_655 ?
O4 Sn2 O3 81.71(6) . 2_655 ?
C29 Sn2 O3 86.67(10) . 2_655 ?
C29 Sn2 O3 160.91(11) 2_655 2_655 ?
O4 Sn2 O3 81.71(6) 2_655 . ?
O4 Sn2 O3 82.87(6) . . ?
C29 Sn2 O3 160.91(11) . . ?
C29 Sn2 O3 86.67(10) 2_655 . ?
O3 Sn2 O3 74.25(8) 2_655 . ?
C1 O1 Sn1 126.96(13) . . ?
C11 O2 Sn1 132.96(14) . . ?
C14 O3 Sn2 130.34(14) . . ?
C15 O4 Sn2 123.38(15) . . ?
C1 N1 N2 111.7(2) . . ?
C1 N1 C5 129.6(2) . . ?
N2 N1 C5 118.4(2) . . ?
C3 N2 N1 105.8(2) . . ?
C15 N3 N4 111.6(2) . . ?
C15 N3 C19 129.1(2) . . ?
N4 N3 C19 118.7(2) . . ?
C17 N4 N3 105.7(2) . . ?
O1 C1 N1 122.3(2) . . ?
O1 C1 C2 131.4(2) . . ?
N1 C1 C2 106.3(2) . . ?
C11 C2 C1 123.0(2) . . ?
C11 C2 C3 132.7(2) . . ?
C1 C2 C3 104.3(2) . . ?
N2 C3 C2 111.9(2) . . ?
N2 C3 C4 118.2(2) . . ?
C2 C3 C4 129.9(2) . . ?
C6 C5 C10 119.8(2) . . ?
C6 C5 N1 120.9(2) . . ?
C10 C5 N1 119.3(2) . . ?
C5 C6 C7 119.4(2) . . ?
C8 C7 C6 121.0(3) . . ?
C9 C8 C7 119.5(2) . . ?
C8 C9 C10 120.6(2) . . ?
C5 C10 C9 119.6(2) . . ?
O2 C11 C2 122.5(2) . . ?
O2 C11 C12 114.7(2) . . ?
C2 C11 C12 122.8(2) . . ?
C11 C12 C13 112.6(2) . . ?
C14 C13 C12 112.4(2) . . ?
O3 C14 C16 122.2(2) . . ?
O3 C14 C13 115.8(2) . . ?
C16 C14 C13 122.0(2) . . ?
O4 C15 N3 122.3(2) . . ?
O4 C15 C16 131.3(2) . . ?
N3 C15 C16 106.4(2) . . ?
C14 C16 C15 123.6(2) . . ?
C14 C16 C17 132.0(2) . . ?
C15 C16 C17 104.3(2) . . ?
N4 C17 C16 111.9(2) . . ?
N4 C17 C18 118.4(2) . . ?
C16 C17 C18 129.7(2) . . ?
C20 C19 C24 120.4(2) . . ?
C20 C19 N3 118.7(2) . . ?
C24 C19 N3 120.8(2) . . ?
C21 C20 C19 119.5(3) . . ?
C20 C21 C22 120.6(3) . . ?
C23 C22 C21 119.5(3) . . ?
C22 C23 C24 120.9(3) . . ?
C23 C24 C19 119.1(3) . . ?
C26 C25 Sn1 110.9(2) . . ?
C27 C26 C25 114.4(2) . . ?
C26 C27 C28 112.4(3) . . ?
C30 C29 Sn2 124.1(3) . . ?
C29 C30 C31 116.1(4) . . ?
C32 C31 C30 128.8(4) . . ?
C29A C30A C31A 110.1(4) . . ?
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
Sn1 O1 2.132(2) . ?
Sn1 O1 2.132(2) 2_655 ?
Sn1 C25 2.143(2) 2_655 ?
Sn1 C25 2.143(2) . ?
Sn1 O2 2.209(2) . ?
Sn1 O2 2.209(2) 2_655 ?
Sn2 O4 2.127(2) 2_655 ?
Sn2 O4 2.127(2) . ?
Sn2 C29 2.132(3) . ?
Sn2 C29 2.132(3) 2_655 ?
Sn2 O3 2.205(2) 2_655 ?
Sn2 O3 2.205(2) . ?
O1 C1 1.275(3) . ?
O2 C11 1.257(3) . ?
O3 C14 1.266(3) . ?
O4 C15 1.284(3) . ?
N1 C1 1.359(3) . ?
N1 N2 1.395(3) . ?
N1 C5 1.424(3) . ?
N2 C3 1.310(3) . ?
N3 C15 1.356(3) . ?
N3 N4 1.397(2) . ?
N3 C19 1.420(3) . ?
N4 C17 1.303(3) . ?
C1 C2 1.421(3) . ?
C2 C11 1.407(3) . ?
C2 C3 1.434(3) . ?
C3 C4 1.491(3) . ?
C5 C6 1.384(3) . ?
C5 C10 1.385(3) . ?
C6 C7 1.386(3) . ?
C7 C8 1.372(4) . ?
C8 C9 1.370(4) . ?
C9 C10 1.389(4) . ?
C11 C12 1.510(3) . ?
C12 C13 1.518(3) . ?
C13 C14 1.501(3) . ?
C14 C16 1.406(3) . ?
C15 C16 1.415(3) . ?
C16 C17 1.436(3) . ?
C17 C18 1.491(3) . ?
C19 C20 1.382(4) . ?
C19 C24 1.386(3) . ?
C20 C21 1.376(4) . ?
C21 C22 1.380(4) . ?
C22 C23 1.373(4) . ?
C23 C24 1.379(4) . ?
C25 C26 1.571(4) . ?
C26 C27 1.487(4) . ?
C27 C28 1.499(4) . ?
C29 C30 1.417(5) . ?
C30 C31 1.506(5) . ?
C31 C32 1.469(5) . ?
C29A C30A 1.319(6) . ?
C30A C31A 1.696(6) . ?
