#------------------------------------------------------------------------------
#$Date: 2019-11-23 07:55:53 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232489 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/77/4347760.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_4347760
loop_
_publ_author_name
'Arras, Janet'
'Eichele, Klaus'
'Maryasin, Boris'
'Schubert, Hartmut'
'Ochsenfeld, Christian'
'Wesemann, Lars'
_publ_section_title
;
 Intermolecular (119)Sn,(31)P Through-Space Spin-Spin Coupling in a Solid
 Bivalent Tin Phosphido Complex.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4669
_journal_page_last               4675
_journal_paper_doi               10.1021/acs.inorgchem.6b00573
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C28 H30 N2 P2 Sn'
_chemical_formula_sum            'C28 H30 N2 P2 Sn'
_chemical_formula_weight         575.19
_chemical_name_common            2(thf)
_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_Hall           'I 4bw -2c'
_space_group_name_H-M_alt        'I 41 c d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.082(2)
_cell_length_b                   21.082(2)
_cell_length_c                   11.5882(12)
_cell_measurement_reflns_used    5738
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      27.5544
_cell_measurement_theta_min      6.9816
_cell_volume                     5150.4(9)
_computing_cell_refinement       'APEX2 v2011.8-0 (Bruker AXS)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17391
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         6.73
_diffrn_source_type              'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.135
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            'clear orange-brown'
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.206
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.017(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2928
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0175
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0268
_refine_ls_wR_factor_ref         0.0279
_reflns_number_gt                2318
_reflns_number_total             2928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00573_si_002.cif
_cod_data_source_block           I
_cod_database_code               4347760
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/2, x, z+3/4'
'y+1/2, -x, z+3/4'
'-x, -y, z'
'-x, y, z+1/2'
'x, -y, z+1/2'
'-y+1/2, -x, z+1/4'
'y+1/2, x, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+1, x+1/2, z+5/4'
'y+1, -x+1/2, z+5/4'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1'
'x+1/2, -y+1/2, z+1'
'-y+1, -x+1/2, z+3/4'
'y+1, x+1/2, z+3/4'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Sn Sn 1.0 1.0 0.50816(3) 0.01375(4) Uani d S 1
P P 0.90309(2) 0.99712(3) 0.36716(4) 0.01700(9) Uani d . 1
N N 0.97776(8) 0.88195(8) 0.44641(13) 0.0157(4) Uani d . 1
C C1 0.87132(10) 0.92798(10) 0.44566(16) 0.0169(5) Uani d . 1
C C2 0.91116(10) 0.87742(10) 0.47779(15) 0.0159(4) Uani d . 1
C C3 0.88683(11) 0.82647(10) 0.53949(15) 0.0205(5) Uani d . 1
H H3 0.9143 0.793 0.5623 0.025 Uiso calc R 1
C C4 0.82314(11) 0.82373(11) 0.56823(16) 0.0224(4) Uani d . 1
H H4 0.8071 0.7885 0.6104 0.027 Uiso calc R 1
C C5 0.78286(11) 0.87226(11) 0.53552(16) 0.0218(5) Uani d . 1
H H5 0.739 0.8705 0.5543 0.026 Uiso calc R 1
C C6 0.80714(10) 0.92347(10) 0.47494(16) 0.0191(5) Uani d . 1
H H6 0.7792 0.9566 0.4525 0.023 Uiso calc R 1
C C7 0.98718(11) 0.87074(10) 0.32048(16) 0.0217(5) Uani d . 1
H H7A 0.9766 0.8266 0.3021 0.033 Uiso calc R 1
H H7B 1.0315 0.879 0.3002 0.033 Uiso calc R 1
H H7C 0.9595 0.8992 0.2764 0.033 Uiso calc R 1
C C8 1.01939(8) 0.83835(9) 0.5101(2) 0.0216(4) Uani d . 1
H H8A 1.0132 0.8444 0.5932 0.032 Uiso calc R 1
H H8B 1.0637 0.8471 0.4902 0.032 Uiso calc R 1
H H8C 1.009 0.7945 0.4893 0.032 Uiso calc R 1
C C9 0.85023(10) 1.05767(10) 0.42736(18) 0.0190(5) Uani d . 1
C C10 0.84014(11) 1.06646(11) 0.54589(18) 0.0213(5) Uani d . 1
H H10 0.8632 1.0415 0.5998 0.026 Uiso calc R 1
C C11 0.79690(11) 1.11107(11) 0.5856(2) 0.0324(6) Uani d . 1
H H11 0.7902 1.1164 0.6661 0.039 Uiso calc R 1
C C12 0.76348(11) 1.14787(11) 0.5069(3) 0.0418(7) Uani d . 1
H H12 0.7332 1.1778 0.5337 0.05 Uiso calc R 1
C C13 0.77389(11) 1.14118(11) 0.3912(3) 0.0385(7) Uani d . 1
H H13 0.7514 1.1671 0.3381 0.046 Uiso calc R 1
C C14 0.81723(10) 1.09651(10) 0.3506(2) 0.0260(5) Uani d . 1
H H14 0.8244 1.0925 0.27 0.031 Uiso calc R 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'
N N 0.0061 0.0033 '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'
H H 0.0000 0.0000 '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_site_symmetry_1
_geom_angle
P Sn P 4_775 102.73(2)
C3 C2 C1 . 120.11(19)
C3 C2 N . 122.45(18)
C1 C2 N . 117.42(18)
C2 N C8 . 114.21(16)
C2 N C7 . 111.28(15)
C8 N C7 . 108.21(16)
C6 C1 C2 . 117.51(19)
C6 C1 P . 121.66(16)
C2 C1 P . 120.82(17)
C11 C10 C9 . 120.9(2)
C11 C10 H10 . 119.5
C9 C10 H10 . 119.5
C14 C9 C10 . 118.1(2)
C14 C9 P . 118.00(16)
C10 C9 P . 123.86(17)
C5 C6 C1 . 122.2(2)
C5 C6 H6 . 118.9
C1 C6 H6 . 118.9
C9 P C1 . 98.16(9)
C9 P Sn . 102.76(7)
C1 P Sn . 89.66(7)
C5 C4 C3 . 119.9(2)
C5 C4 H4 . 120.0
C3 C4 H4 . 120.0
C4 C5 C6 . 119.2(2)
C4 C5 H5 . 120.4
C6 C5 H5 . 120.4
C4 C3 C2 . 120.9(2)
C4 C3 H3 . 119.5
C2 C3 H3 . 119.5
N C7 H7A . 109.5
N C7 H7B . 109.5
H7A C7 H7B . 109.5
N C7 H7C . 109.5
H7A C7 H7C . 109.5
H7B C7 H7C . 109.5
N C8 H8A . 109.5
N C8 H8B . 109.5
H8A C8 H8B . 109.5
N C8 H8C . 109.5
H8A C8 H8C . 109.5
H8B C8 H8C . 109.5
C13 C12 C11 . 120.4(2)
C13 C12 H12 . 119.8
C11 C12 H12 . 119.8
C12 C13 C14 . 120.4(2)
C12 C13 H13 . 119.8
C14 C13 H13 . 119.8
C13 C14 C9 . 120.5(2)
C13 C14 H14 . 119.7
C9 C14 H14 . 119.7
C10 C11 C12 . 119.6(2)
C10 C11 H11 . 120.2
C12 C11 H11 . 120.2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Sn P 4_775 2.6167(5)
Sn P . 2.6167(5)
C2 C3 . 1.388(3)
C2 C1 . 1.407(3)
C2 N . 1.454(3)
N C8 . 1.470(2)
N C7 . 1.492(2)
C1 C6 . 1.398(3)
C1 P . 1.844(2)
C10 C11 . 1.388(3)
C10 C9 . 1.402(3)
C10 H10 . 0.95
C9 C14 . 1.395(3)
C9 P . 1.833(2)
C6 C5 . 1.386(3)
C6 H6 . 0.95
C5 C4 . 1.383(3)
C4 C3 . 1.385(3)
C4 H4 . 0.95
C5 H5 . 0.95
C3 H3 . 0.95
C7 H7A . 0.98
C7 H7B . 0.98
C7 H7C . 0.98
C8 H8A . 0.98
C8 H8B . 0.98
C8 H8C . 0.98
C12 C13 . 1.366(4)
C12 C11 . 1.389(4)
C12 H12 . 0.95
C13 C14 . 1.394(3)
C13 H13 . 0.95
C14 H14 . 0.95
C11 H11 . 0.95
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion
C3 C2 N C8 . -15.4(2)
C1 C2 N C8 . 163.01(17)
C3 C2 N C7 . 107.4(2)
C1 C2 N C7 . -74.1(2)
C3 C2 C1 C6 . -2.0(3)
N C2 C1 C6 . 179.49(16)
C3 C2 C1 P . 178.32(14)
N C2 C1 P . -0.2(2)
C11 C10 C9 C14 . 2.2(4)
C11 C10 C9 P . -176.61(16)
C2 C1 C6 C5 . 1.4(3)
P C1 C6 C5 . -178.95(15)
C14 C9 P C1 . -127.39(17)
C10 C9 P C1 . 51.4(2)
C14 C9 P Sn . 141.11(16)
C10 C9 P Sn . -40.1(2)
C6 C1 P C9 . 32.82(18)
C2 C1 P C9 . -147.53(16)
C6 C1 P Sn . 135.67(16)
C2 C1 P Sn . -44.68(15)
P Sn P C9 4_775 -132.90(7)
P Sn P C1 4_775 128.81(7)
C3 C4 C5 C6 . -0.6(3)
C1 C6 C5 C4 . -0.1(3)
C5 C4 C3 C2 . -0.1(3)
C1 C2 C3 C4 . 1.4(3)
N C2 C3 C4 . 179.83(17)
C11 C12 C13 C14 . 1.3(3)
C12 C13 C14 C9 . 0.5(3)
C10 C9 C14 C13 . -2.2(3)
P C9 C14 C13 . 176.67(16)
C9 C10 C11 C12 . -0.5(4)
C13 C12 C11 C10 . -1.3(3)
