#------------------------------------------------------------------------------
#$Date: 2016-03-21 14:42:33 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178720 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/31/4083161.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_4083161
loop_
_publ_author_name
'Hupf, Emanuel'
'Lork, Enno'
'Mebs, Stefan'
'Beckmann, Jens'
_publ_section_title
;
 Intramolecularly Coordinated
 (6-(Diphenylphosphino)acenaphth-5-yl)stannanes. Repulsion vs Attraction
 of P- and Sn-Containing Substituents in theperiPositions
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2409
_journal_paper_doi               10.1021/om500133a
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C48 H36 Cl2 P2 Sn'
_chemical_formula_sum            'C48 H36 Cl2 P2 Sn'
_chemical_formula_weight         864.30
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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     iterative
_audit_creation_date             2013-08-29
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.95(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.628(8)
_cell_length_b                   16.015(8)
_cell_length_c                   17.472(11)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    173
_cell_measurement_theta_max      12.46
_cell_measurement_theta_min      2.77
_cell_volume                     3756(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '2θ/ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10009
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_min         2.544
_diffrn_source                   'normal-focus sealed tube'
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.944
_exptl_absorpt_correction_T_max  0.794
_exptl_absorpt_correction_T_min  0.397
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'Walker & Stuart, Acta Cyst A, 1983'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         4326
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0334P)²+3.6348P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3546
_reflns_number_total             4326
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om500133a_si_002.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 4083156--4083163.cif.'
_cod_database_code               4083161
#BEGIN Tags that were not found in dictionaries:
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C16(H16), C17(H17), C21(H21), C22(H22), C23(H23),
 C24(H24), C25(H25), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35)
;
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Sn1 Sn 0.5000 0.31678(2) 0.7500 0.01871(9) Uani 1 2 d S T P
Cl1 Cl 0.40837(5) 0.20860(5) 0.80659(4) 0.02786(16) Uani 1 1 d . . .
P1 P 0.35178(5) 0.41988(5) 0.80746(4) 0.01983(16) Uani 1 1 d . . .
C1 C 0.1644(2) 0.3775(2) 0.44611(17) 0.0303(7) Uani 1 1 d . . .
H1A H 0.1493 0.3278 0.4125 0.036 Uiso 1 1 calc R U .
H1B H 0.1763 0.4257 0.4134 0.036 Uiso 1 1 calc R U .
C2 C 0.0783(2) 0.3960(2) 0.49039(18) 0.0350(8) Uani 1 1 d . . .
H2A H 0.0437 0.4483 0.4714 0.042 Uiso 1 1 calc R U .
H2B H 0.0294 0.3497 0.4838 0.042 Uiso 1 1 calc R U .
C10 C 0.3938(2) 0.34856(17) 0.64882(15) 0.0191(5) Uani 1 1 d . . .
C11 C 0.4180(2) 0.33098(18) 0.57668(16) 0.0250(6) Uani 1 1 d . . .
H11 H 0.4837 0.3126 0.5745 0.030 Uiso 1 1 calc R U .
C12 C 0.3496(2) 0.33907(19) 0.50580(16) 0.0272(7) Uani 1 1 d . . .
H12 H 0.3701 0.3289 0.4574 0.033 Uiso 1 1 calc R U .
C13 C 0.2542(2) 0.36177(18) 0.50893(16) 0.0240(6) Uani 1 1 d . . .
C14 C 0.2281(2) 0.37991(17) 0.58171(16) 0.0218(6) Uani 1 1 d . . .
C15 C 0.1274(2) 0.40456(19) 0.57522(17) 0.0264(6) Uani 1 1 d . . .
C16 C 0.0928(2) 0.4296(2) 0.64036(18) 0.0290(7) Uani 1 1 d . . .
H16 H 0.0250 0.4449 0.6378 0.035 Uiso 1 1 calc R U .
C17 C 0.1603(2) 0.43221(19) 0.71202(17) 0.0266(6) Uani 1 1 d . . .
H17 H 0.1364 0.4514 0.7569 0.032 Uiso 1 1 calc R U .
C18 C 0.2590(2) 0.40828(18) 0.71991(16) 0.0215(6) Uani 1 1 d . . .
C19 C 0.2960(2) 0.37764(17) 0.65262(15) 0.0188(5) Uani 1 1 d . . .
C20 C 0.2875(2) 0.40026(18) 0.88919(16) 0.0210(6) Uani 1 1 d . . .
C21 C 0.2111(2) 0.3408(2) 0.88457(18) 0.0294(7) Uani 1 1 d . . .
H21 H 0.1894 0.3115 0.8374 0.035 Uiso 1 1 calc R U .
C22 C 0.1676(2) 0.3253(2) 0.94874(19) 0.0355(8) Uani 1 1 d . . .
H22 H 0.1154 0.2853 0.9450 0.043 Uiso 1 1 calc R U .
C23 C 0.1980(2) 0.3665(2) 1.01852(18) 0.0318(7) Uani 1 1 d . . .
H23 H 0.1671 0.3553 1.0622 0.038 Uiso 1 1 calc R U .
C24 C 0.2740(2) 0.42410(19) 1.02346(17) 0.0281(7) Uani 1 1 d . . .
H24 H 0.2960 0.4526 1.0710 0.034 Uiso 1 1 calc R U .
C25 C 0.3183(2) 0.44080(19) 0.95943(17) 0.0258(6) Uani 1 1 d . . .
H25 H 0.3707 0.4806 0.9637 0.031 Uiso 1 1 calc R U .
C30 C 0.3798(2) 0.53165(18) 0.81318(15) 0.0211(6) Uani 1 1 d . . .
C31 C 0.3114(2) 0.59430(19) 0.78719(16) 0.0254(6) Uani 1 1 d . . .
H31 H 0.2448 0.5800 0.7652 0.031 Uiso 1 1 calc R U .
C32 C 0.3396(2) 0.67731(19) 0.79313(18) 0.0286(6) Uani 1 1 d . . .
H32 H 0.2924 0.7197 0.7753 0.034 Uiso 1 1 calc R U .
C33 C 0.4365(2) 0.69901(19) 0.82496(18) 0.0296(7) Uani 1 1 d . . .
H33 H 0.4554 0.7561 0.8290 0.035 Uiso 1 1 calc R U .
C34 C 0.5056(2) 0.63768(19) 0.85081(18) 0.0278(6) Uani 1 1 d . . .
H34 H 0.5723 0.6525 0.8720 0.033 Uiso 1 1 calc R U .
C35 C 0.4775(2) 0.55453(19) 0.84573(16) 0.0250(6) Uani 1 1 d . . .
H35 H 0.5248 0.5125 0.8645 0.030 Uiso 1 1 calc R U .
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'
Cl Cl 0.1484 0.1585 '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'
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
Cl1 Sn1 Cl1 89.64(6) 2_656 .
Cl1 Sn1 P1 166.75(3) 2_656 .
Cl1 Sn1 P1 80.17(5) . .
Cl1 Sn1 P1 166.75(3) . 2_656
Cl1 Sn1 P1 80.17(5) 2_656 2_656
P1 Sn1 P1 111.08(5) 2_656 .
C10 Sn1 Cl1 98.87(8) . 2_656
C10 Sn1 Cl1 98.87(9) 2_656 .
C10 Sn1 Cl1 100.52(8) 2_656 2_656
C10 Sn1 Cl1 100.52(8) . .
C10 Sn1 P1 89.48(9) 2_656 .
C10 Sn1 P1 74.95(9) . .
C10 Sn1 P1 74.95(9) 2_656 2_656
C10 Sn1 P1 89.48(9) . 2_656
C10 Sn1 C10 152.54(15) . 2_656
C18 P1 Sn1 94.28(10) . .
C18 P1 C20 106.43(14) . .
C18 P1 C30 104.72(13) . .
C20 P1 Sn1 128.71(10) . .
C20 P1 C30 104.43(13) . .
C30 P1 Sn1 114.98(9) . .
C13 C1 C2 104.9(2) . .
C15 C2 C1 105.2(3) . .
C11 C10 Sn1 118.0(2) . .
C11 C10 C19 118.7(3) . .
C19 C10 Sn1 122.9(2) . .
C10 C11 C12 123.4(3) . .
C13 C12 C11 118.5(3) . .
C12 C13 C1 132.3(3) . .
C12 C13 C14 118.9(3) . .
C14 C13 C1 108.7(3) . .
C13 C14 C15 112.2(3) . .
C13 C14 C19 123.8(3) . .
C15 C14 C19 123.9(3) . .
C14 C15 C2 108.1(3) . .
C16 C15 C2 132.9(3) . .
C16 C15 C14 119.1(3) . .
C15 C16 C17 118.6(3) . .
C18 C17 C16 123.4(3) . .
C17 C18 P1 125.4(2) . .
C17 C18 C19 118.9(3) . .
C19 C18 P1 115.5(2) . .
C10 C19 C18 127.7(3) . .
C14 C19 C10 116.4(3) . .
C14 C19 C18 115.9(2) . .
C21 C20 P1 121.5(2) . .
C25 C20 P1 119.9(2) . .
C25 C20 C21 118.4(3) . .
C22 C21 C20 119.7(3) . .
C21 C22 C23 121.6(3) . .
C24 C23 C22 118.8(3) . .
C23 C24 C25 120.4(3) . .
C24 C25 C20 121.1(3) . .
C31 C30 P1 124.5(2) . .
C31 C30 C35 118.6(3) . .
C35 C30 P1 116.9(2) . .
C32 C31 C30 120.4(3) . .
C31 C32 C33 120.3(3) . .
C34 C33 C32 120.1(3) . .
C33 C34 C35 119.8(3) . .
C34 C35 C30 120.7(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 Cl1 2.4424(13) 2_656
Sn1 Cl1 2.4424(13) .
Sn1 P1 2.9182(16) 2_656
Sn1 P1 2.9182(16) .
Sn1 C10 2.144(3) .
Sn1 C10 2.144(3) 2_656
P1 C18 1.818(3) .
P1 C20 1.826(3) .
P1 C30 1.829(3) .
C1 C2 1.541(5) .
C1 C13 1.517(4) .
C2 C15 1.523(4) .
C10 C11 1.386(4) .
C10 C19 1.424(4) .
C11 C12 1.421(4) .
C12 C13 1.360(4) .
C13 C14 1.409(4) .
C14 C15 1.413(4) .
C14 C19 1.413(4) .
C15 C16 1.366(4) .
C16 C17 1.421(4) .
C17 C18 1.382(4) .
C18 C19 1.443(4) .
C20 C21 1.403(4) .
C20 C25 1.388(4) .
C21 C22 1.379(4) .
C22 C23 1.386(5) .
C23 C24 1.377(5) .
C24 C25 1.387(4) .
C30 C31 1.391(4) .
C30 C35 1.403(4) .
C31 C32 1.383(4) .
C32 C33 1.385(4) .
C33 C34 1.382(4) .
C34 C35 1.384(4) .
