#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:20:33 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178646 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/57/4075785.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_4075785
loop_
_publ_author_name
'Nemes, Gabriela Cretiu'
'Silaghi-Dumitrescu, Luminita'
'Silaghi-Dumitrescu, Ioan'
'Escudié, Jean'
'Ranaivonjatovo, Henri'
'Molloy, Kieran C.'
'Mahon, Mary F.'
'Zukerman-Schpector, Julio'
_publ_section_title
;
 Difluorenylsilanes, -germanes, and -stannanes Exhibiting an Unprecedented
 Parallel Arrangement of the Fluorene Units
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1134
_journal_paper_doi               10.1021/om049543y
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C30 H28 Sn'
_chemical_formula_weight         507.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 117.517(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.377(4)
_cell_length_b                   13.344(2)
_cell_length_c                   18.147(4)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      11.9
_cell_measurement_theta_min      5.09
_cell_volume                     4805.7(17)
_computing_cell_refinement       'Siemens (Bruker) P3-P4/PC'
_computing_data_collection       'Siemens (Bruker) P3-P4/PC'
_computing_data_reduction        'Siemens (Bruker) Xdisk'
_computing_molecular_graphics    'ZORTEP (Zsolnai, 1995)'
_computing_publication_material  PARST95-Nardelli,PLATON-Spek,WinGX-Farrugia
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  Saxi/P3
_diffrn_measurement_method       'Wyckoff omega-scan'
_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  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3252
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.53
_diffrn_standards_interval_count 100
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_T_max  0.551
_exptl_absorpt_correction_T_min  0.506
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3132
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0317
_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)+(0.0509P)²+6.5016P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0857
_reflns_number_gt                2695
_reflns_number_total             3132
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om049543ysi20041215_103715.cif
_cod_data_source_block           4c
_cod_depositor_comments
;
The following automatic conversions were performed:
'__exptl_crystal_description' tag replaced with
'_exptl_crystal_description'.

'__computing_data_collection' tag
replaced with '_computing_data_collection'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_cell_volume        4805.7(16)
_cod_database_code               4075785
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Sn Sn 0.162743(13) 0.77303(2) 0.138893(17) 0.04284(14) Uani 1 1 d .
C1 C 0.0789(2) 0.7101(4) -0.0873(3) 0.0542(12) Uani 1 1 d .
H1 H 0.1127 0.7537 -0.0867 0.065 Uiso 1 1 calc R
C2 C 0.0567(2) 0.6297(4) -0.1418(3) 0.0652(14) Uani 1 1 d .
H2 H 0.0746 0.6194 -0.1796 0.078 Uiso 1 1 calc R
C3 C 0.0095(3) 0.5652(4) -0.1416(3) 0.0651(14) Uani 1 1 d .
H3 H -0.0040 0.5094 -0.1782 0.078 Uiso 1 1 calc R
C4 C -0.0190(2) 0.5795(3) -0.0893(3) 0.0544(11) Uani 1 1 d .
H4 H -0.0523 0.5346 -0.0901 0.065 Uiso 1 1 calc R
C5 C -0.0695(2) 0.6606(4) 0.0439(3) 0.0556(12) Uani 1 1 d .
H5 H -0.0934 0.6007 0.0192 0.067 Uiso 1 1 calc R
C6 C -0.0811(3) 0.7117(4) 0.1016(3) 0.0659(14) Uani 1 1 d .
H6 H -0.1123 0.6855 0.1185 0.079 Uiso 1 1 calc R
C7 C -0.0485(2) 0.8003(4) 0.1354(3) 0.0660(14) Uani 1 1 d .
H7 H -0.0582 0.8347 0.1745 0.079 Uiso 1 1 calc R
C8 C -0.0015(2) 0.8403(4) 0.1134(3) 0.0533(11) Uani 1 1 d .
H8 H 0.0203 0.9021 0.1361 0.064 Uiso 1 1 calc R
C9 C 0.06476(19) 0.8081(3) 0.0286(2) 0.0438(10) Uani 1 1 d .
C10 C 0.0513(2) 0.7264(3) -0.0336(2) 0.0423(10) Uani 1 1 d .
C11 C 0.0127(2) 0.7874(3) 0.0572(2) 0.0433(10) Uani 1 1 d .
C12 C -0.0218(2) 0.6986(3) 0.0224(3) 0.0436(10) Uani 1 1 d .
C13 C 0.0019(2) 0.6606(3) -0.0355(2) 0.0427(10) Uani 1 1 d .
C1' C 0.2692(2) 0.9576(4) 0.1071(4) 0.0719(15) Uani 1 1 d .
H1' H 0.2971 0.8999 0.1198 0.086 Uiso 1 1 calc R
C2' C 0.2683(3) 1.0263(5) 0.0498(4) 0.0872(19) Uani 1 1 d .
H2' H 0.2955 1.0155 0.0230 0.105 Uiso 1 1 calc R
C3' C 0.2286(3) 1.1095(5) 0.0311(4) 0.0822(17) Uani 1 1 d .
H3' H 0.2282 1.1554 -0.0092 0.099 Uiso 1 1 calc R
C4' C 0.1891(3) 1.1286(4) 0.0693(3) 0.0617(13) Uani 1 1 d .
H4' H 0.1616 1.1868 0.0559 0.074 Uiso 1 1 calc R
C5' C 0.1114(2) 1.1311(4) 0.1851(3) 0.0571(12) Uani 1 1 d .
H5' H 0.0970 1.1879 0.1495 0.069 Uiso 1 1 calc R
C6' C 0.0892(3) 1.1157(5) 0.2432(4) 0.0769(17) Uani 1 1 d .
H6' H 0.0596 1.1629 0.2486 0.092 Uiso 1 1 calc R
C7' C 0.1092(3) 1.0331(5) 0.2934(4) 0.0821(18) Uani 1 1 d .
H7' H 0.0939 1.0248 0.3339 0.098 Uiso 1 1 calc R
C8' C 0.1507(2) 0.9618(4) 0.2870(3) 0.0631(13) Uani 1 1 d .
H8' H 0.1636 0.9046 0.3221 0.076 Uiso 1 1 calc R
C9' C 0.2184(2) 0.9095(3) 0.2074(3) 0.0484(11) Uani 1 1 d .
C10' C 0.22932(19) 0.9730(3) 0.1461(3) 0.0465(10) Uani 1 1 d .
C11' C 0.1737(2) 0.9748(3) 0.2279(2) 0.0450(10) Uani 1 1 d .
C12' C 0.15575(19) 1.0616(3) 0.1792(2) 0.0428(10) Uani 1 1 d .
C13' C 0.1904(2) 1.0609(3) 0.1279(2) 0.0442(10) Uani 1 1 d .
C14 C 0.2268(3) 0.6929(5) 0.1009(3) 0.0766(16) Uani 1 1 d .
H14A H 0.2718 0.6861 0.1482 0.115 Uiso 1 1 calc R
H14B H 0.2301 0.7297 0.0562 0.115 Uiso 1 1 calc R
H14C H 0.2079 0.6262 0.0809 0.115 Uiso 1 1 calc R
C15 C 0.1423(3) 0.6816(4) 0.2216(3) 0.0673(13) Uani 1 1 d .
H15A H 0.1253 0.6162 0.1958 0.101 Uiso 1 1 calc R
H15B H 0.1084 0.7144 0.2333 0.101 Uiso 1 1 calc R
H15C H 0.1839 0.6722 0.2737 0.101 Uiso 1 1 calc R
C16 C 0.0653(2) 0.9135(3) -0.0048(3) 0.0542(11) Uani 1 1 d .
H16A H 0.1040 0.9202 -0.0161 0.081 Uiso 1 1 calc R
H16B H 0.0687 0.9635 0.0365 0.081 Uiso 1 1 calc R
H16C H 0.0235 0.9243 -0.0563 0.081 Uiso 1 1 calc R
C17 C 0.2831(2) 0.8735(4) 0.2827(3) 0.0794(16) Uani 1 1 d .
H17A H 0.3074 0.9314 0.3165 0.119 Uiso 1 1 calc R
H17B H 0.3118 0.8387 0.2633 0.119 Uiso 1 1 calc R
H17C H 0.2714 0.8276 0.3161 0.119 Uiso 1 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'
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
C15 Sn C14 109.4(2)
C15 Sn C9 108.00(17)
C14 Sn C9 110.01(18)
C15 Sn C9' 108.62(19)
C14 Sn C9' 107.6(2)
C9 Sn C9' 113.15(15)
C2 C1 C10 119.5(4)
C3 C2 C1 120.6(4)
C2 C3 C4 121.4(5)
C3 C4 C13 118.6(4)
C6 C5 C12 118.2(5)
C5 C6 C7 121.4(4)
C6 C7 C8 121.0(4)
C11 C8 C7 118.3(4)
C10 C9 C11 102.1(3)
C10 C9 C16 114.0(3)
C11 C9 C16 116.9(4)
C10 C9 Sn 107.2(3)
C11 C9 Sn 104.4(3)
C16 C9 Sn 111.3(3)
C1 C10 C13 119.1(4)
C1 C10 C9 130.0(4)
C13 C10 C9 110.9(4)
C8 C11 C12 119.8(4)
C8 C11 C9 129.4(4)
C12 C11 C9 110.7(3)
C5 C12 C11 121.2(4)
C5 C12 C13 130.7(4)
C11 C12 C13 108.1(4)
C4 C13 C10 120.9(4)
C4 C13 C12 131.0(4)
C10 C13 C12 107.9(4)
C2' C1' C10' 119.8(5)
C3' C2' C1' 120.7(5)
C2' C3' C4' 121.4(5)
C3' C4' C13' 118.4(5)
C6' C5' C12' 118.7(5)
C7' C6' C5' 120.6(5)
C6' C7' C8' 122.0(5)
C7' C8' C11' 118.9(5)
C11' C9' C10' 102.2(3)
C11' C9' C17 115.1(4)
C10' C9' C17 115.1(4)
C11' C9' Sn 110.4(3)
C10' C9' Sn 106.7(3)
C17 C9' Sn 107.1(3)
C1' C10' C13' 118.7(4)
C1' C10' C9' 131.0(4)
C13' C10' C9' 110.3(4)
C8' C11' C12' 119.1(4)
C8' C11' C9' 130.0(4)
C12' C11' C9' 110.8(4)
C5' C12' C11' 120.6(4)
C5' C12' C13' 131.1(4)
C11' C12' C13' 108.3(4)
C4' C13' C10' 120.9(4)
C4' C13' C12' 131.0(4)
C10' C13' C12' 108.1(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Sn C15 2.142(5)
Sn C14 2.142(5)
Sn C9 2.231(4)
Sn C9' 2.232(4)
C1 C2 1.386(7)
C1 C10 1.392(6)
C2 C3 1.364(7)
C3 C4 1.380(7)
C4 C13 1.387(6)
C5 C6 1.372(7)
C5 C12 1.391(6)
C6 C7 1.375(7)
C7 C8 1.393(7)
C8 C11 1.391(6)
C9 C10 1.495(6)
C9 C11 1.505(6)
C9 C16 1.535(6)
C10 C13 1.399(6)
C11 C12 1.395(6)
C12 C13 1.468(5)
C1' C2' 1.379(8)
C1' C10' 1.387(6)
C2' C3' 1.363(9)
C3' C4' 1.377(8)
C4' C13' 1.385(6)
C5' C6' 1.375(7)
C5' C12' 1.397(6)
C6' C7' 1.366(8)
C7' C8' 1.372(8)
C8' C11' 1.398(6)
C9' C11' 1.497(6)
C9' C10' 1.506(6)
C9' C17 1.538(6)
C10' C13' 1.407(6)
C11' C12' 1.399(6)
C12' C13' 1.460(6)
