#------------------------------------------------------------------------------
#$Date: 2019-11-26 15:51:27 +0100 (mar 26 de nov de 2019) $
#$Revision: 243666 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/95/4089521.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_4089521
loop_
_publ_author_name
'Chandrasekhar, Vadapalli'
'Metre, Ramesh K.'
'Biswas, Sourav'
_publ_section_title
;
 Stabilizing the [RSn(μ2-O)SnR] Motif through Intramolecular
 N→ Sn Coordination. Synthesis and Characterization of
 [(RSn)2(μ2-O)(μ2-FcCOO)2(η-FcCOO)2]·THF and
 {(RSn)2(μ2-O)[(t-BuO)2PO2]2Cl2}·THF·2H2O (R =
 2-(Phenylazo)phenyl)
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              3419
_journal_paper_doi               10.1021/om400346b
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C12 H9 Cl3 N2 Sn'
_chemical_formula_sum            'C12 H9 Cl3 N2 Sn'
_chemical_formula_weight         406.27
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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-97
_cell_angle_alpha                106.694(2)
_cell_angle_beta                 102.640(3)
_cell_angle_gamma                101.147(3)
_cell_formula_units_Z            2
_cell_length_a                   7.0592(11)
_cell_length_b                   9.4325(15)
_cell_length_c                   11.7653(19)
_cell_measurement_reflns_used    2565
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.45
_cell_volume                     704.16(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3845
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    2.365
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.792086
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            color
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             392.0
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0453P)²+0.5230P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0785
_reflns_number_gt                2391
_reflns_number_total             2577
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400346b_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        ' C12 H9 Cl3 N2 Sn'
_cod_database_code               4089521
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Sn1 Sn 0.79157(4) 0.66272(3) 0.26388(2) 0.01737(11) Uani 1 1 d .
Cl3 Cl 1.09136(14) 0.82361(10) 0.40918(8) 0.0229(2) Uani 1 1 d .
Cl2 Cl 0.52629(14) 0.77207(11) 0.27949(9) 0.0256(2) Uani 1 1 d .
Cl1 Cl 0.85246(17) 0.73120(11) 0.09267(9) 0.0295(2) Uani 1 1 d .
N1 N 0.7500(4) 0.5608(3) 0.4291(3) 0.0156(6) Uani 1 1 d .
C1 C 0.7499(5) 0.6343(4) 0.5534(3) 0.0169(7) Uani 1 1 d .
N2 N 0.7478(4) 0.4208(3) 0.4014(3) 0.0179(6) Uani 1 1 d .
C7 C 0.7442(5) 0.3468(4) 0.2766(3) 0.0160(7) Uani 1 1 d .
C5 C 0.7527(6) 0.6342(4) 0.7574(3) 0.0207(8) Uani 1 1 d .
H5 H 0.7513 0.5829 0.8140 0.025 Uiso 1 1 calc R
C2 C 0.7543(6) 0.7887(4) 0.5893(3) 0.0203(8) Uani 1 1 d .
H2 H 0.7542 0.8402 0.5327 0.024 Uiso 1 1 calc R
C6 C 0.7483(5) 0.5558(4) 0.6374(3) 0.0189(7) Uani 1 1 d .
H6 H 0.7443 0.4520 0.6131 0.023 Uiso 1 1 calc R
C3 C 0.7588(6) 0.8660(4) 0.7096(3) 0.0227(8) Uani 1 1 d .
H3 H 0.7615 0.9695 0.7340 0.027 Uiso 1 1 calc R
C10 C 0.7267(6) 0.1857(5) 0.0361(4) 0.0249(8) Uani 1 1 d .
H10 H 0.7176 0.1306 -0.0453 0.030 Uiso 1 1 calc R
C11 C 0.7240(6) 0.1107(5) 0.1216(4) 0.0245(8) Uani 1 1 d .
H11 H 0.7164 0.0064 0.0976 0.029 Uiso 1 1 calc R
C12 C 0.7325(6) 0.1899(4) 0.2425(4) 0.0216(8) Uani 1 1 d .
H12 H 0.7304 0.1397 0.2998 0.026 Uiso 1 1 calc R
C9 C 0.7429(6) 0.3430(4) 0.0710(3) 0.0235(8) Uani 1 1 d .
H9 H 0.7474 0.3930 0.0137 0.028 Uiso 1 1 calc R
C8 C 0.7522(5) 0.4245(4) 0.1920(3) 0.0171(7) Uani 1 1 d .
C4 C 0.7592(5) 0.7889(5) 0.7938(3) 0.0219(8) Uani 1 1 d .
H4 H 0.7639 0.8412 0.8749 0.026 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sn1 0.02291(17) 0.01618(16) 0.01631(16) 0.00729(11) 0.00764(11) 0.00791(11)
Cl3 0.0237(5) 0.0192(5) 0.0246(5) 0.0076(4) 0.0073(4) 0.0032(4)
Cl2 0.0288(5) 0.0289(5) 0.0264(5) 0.0131(4) 0.0099(4) 0.0163(4)
Cl1 0.0499(6) 0.0266(5) 0.0212(5) 0.0141(4) 0.0173(4) 0.0145(4)
N1 0.0155(15) 0.0176(16) 0.0141(14) 0.0066(12) 0.0047(11) 0.0030(12)
C1 0.0152(17) 0.0210(19) 0.0142(17) 0.0054(14) 0.0051(13) 0.0043(14)
N2 0.0182(15) 0.0177(16) 0.0191(15) 0.0083(12) 0.0049(12) 0.0051(12)
C7 0.0112(16) 0.0195(18) 0.0159(16) 0.0051(14) 0.0021(13) 0.0042(14)
C5 0.0212(18) 0.027(2) 0.0186(18) 0.0116(16) 0.0092(15) 0.0065(15)
C2 0.0247(19) 0.0219(19) 0.0194(18) 0.0105(15) 0.0099(15) 0.0090(16)
C6 0.0152(17) 0.0190(18) 0.0224(18) 0.0068(15) 0.0061(14) 0.0042(14)
C3 0.030(2) 0.0188(19) 0.0210(19) 0.0053(15) 0.0102(16) 0.0090(16)
C10 0.025(2) 0.027(2) 0.0196(19) 0.0026(16) 0.0057(15) 0.0086(17)
C11 0.0209(19) 0.022(2) 0.026(2) 0.0026(16) 0.0052(16) 0.0058(16)
C12 0.0187(18) 0.0203(19) 0.029(2) 0.0124(16) 0.0090(15) 0.0059(15)
C9 0.027(2) 0.024(2) 0.0184(19) 0.0044(16) 0.0057(15) 0.0092(16)
C8 0.0181(18) 0.0138(17) 0.0195(18) 0.0053(14) 0.0061(14) 0.0046(14)
C4 0.0192(19) 0.032(2) 0.0147(17) 0.0078(16) 0.0060(14) 0.0062(16)
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'
Cl Cl 0.1484 0.1585 '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
C8 Sn1 Cl3 120.53(10)
C8 Sn1 Cl2 123.31(10)
Cl3 Sn1 Cl2 110.95(4)
C8 Sn1 Cl1 99.58(10)
Cl3 Sn1 Cl1 96.34(4)
Cl2 Sn1 Cl1 96.65(3)
C8 Sn1 N1 73.00(12)
Cl3 Sn1 N1 84.38(7)
Cl2 Sn1 N1 90.92(7)
Cl1 Sn1 N1 171.56(7)
N2 N1 C1 115.2(3)
N2 N1 Sn1 112.7(2)
C1 N1 Sn1 131.7(2)
C2 C1 C6 120.5(3)
C2 C1 N1 117.7(3)
C6 C1 N1 121.9(3)
N1 N2 C7 115.1(3)
C12 C7 C8 121.2(3)
C12 C7 N2 116.0(3)
C8 C7 N2 122.9(3)
C6 C5 C4 120.4(3)
C3 C2 C1 119.9(3)
C5 C6 C1 119.1(3)
C2 C3 C4 119.9(4)
C11 C10 C9 120.6(3)
C12 C11 C10 120.6(4)
C11 C12 C7 118.7(3)
C8 C9 C10 119.6(3)
C9 C8 C7 119.3(3)
C9 C8 Sn1 125.0(3)
C7 C8 Sn1 115.6(3)
C5 C4 C3 120.2(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Sn1 C8 2.099(3)
Sn1 Cl3 2.3213(10)
Sn1 Cl2 2.3223(10)
Sn1 Cl1 2.3830(10)
Sn1 N1 2.451(3)
N1 N2 1.262(4)
N1 C1 1.426(4)
C1 C2 1.388(5)
C1 C6 1.396(5)
N2 C7 1.425(4)
C7 C12 1.398(5)
C7 C8 1.400(5)
C5 C6 1.383(5)
C5 C4 1.386(5)
C2 C3 1.384(5)
C3 C4 1.387(5)
C10 C11 1.388(6)
C10 C9 1.396(6)
C11 C12 1.385(5)
C9 C8 1.390(5)
