#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/69/1506941.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_1506941
loop_
_publ_author_name
'Dai, Weixiang'
'Petersen, Jeffrey L.'
'Wang, Kung K.'
_publ_section_title
;
 Synthesis and structure of a helical diindenophenanthrene with four
 congested phenyl substituents as a molecular spiral staircase.
;
_journal_issue                   23
_journal_name_full               'Organic letters'
_journal_page_first              4355
_journal_page_last               4357
_journal_paper_doi               10.1021/ol0481434
_journal_volume                  6
_journal_year                    2004
_chemical_formula_sum            'C60 H50'
_chemical_formula_weight         771.00
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.230(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.496(3)
_cell_length_b                   10.8830(16)
_cell_length_c                   20.523(3)
_cell_measurement_temperature    223(2)
_cell_volume                     4174.5(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0602
_diffrn_reflns_av_sigmaI/netI    0.0786
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14565
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       0.0009(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         4724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0489
_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)+(0.0505P)²+0.9703P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1296
_reflns_number_gt                2552
_reflns_number_total             4724
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol0481434si20040914_101438.cif
_cod_data_source_block           wd9ccd
_cod_original_cell_volume        4174.5(10)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               1506941
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
C1 C 0.49743(11) 0.80296(17) 0.28149(10) 0.0371(5) Uani 1 1 d .
H1 H 0.5020 0.8776 0.3060 0.045 Uiso 1 1 calc R
C2 C 0.48513(10) 0.69179(17) 0.31247(9) 0.0324(5) Uani 1 1 d .
C3 C 0.47020(10) 0.68892(17) 0.37516(9) 0.0328(4) Uani 1 1 d .
C4 C 0.42808(10) 0.59148(17) 0.37805(9) 0.0322(4) Uani 1 1 d .
C5 C 0.39631(11) 0.56059(18) 0.43152(10) 0.0386(5) Uani 1 1 d .
H5A H 0.4325 0.5247 0.4752 0.046 Uiso 1 1 calc R
H5B H 0.3762 0.6339 0.4441 0.046 Uiso 1 1 calc R
C6 C 0.33910(11) 0.46955(18) 0.39257(10) 0.0375(5) Uani 1 1 d .
C7 C 0.28731(13) 0.42121(19) 0.41275(12) 0.0485(6) Uani 1 1 d .
H7 H 0.2895 0.4354 0.4588 0.058 Uiso 1 1 calc R
C8 C 0.23266(13) 0.3520(2) 0.36385(13) 0.0539(6) Uani 1 1 d .
H8 H 0.1989 0.3145 0.3776 0.065 Uiso 1 1 calc R
C9 C 0.22705(12) 0.33715(19) 0.29503(12) 0.0469(6) Uani 1 1 d .
H9 H 0.1877 0.2941 0.2618 0.056 Uiso 1 1 calc R
C10 C 0.27849(11) 0.38465(17) 0.27338(11) 0.0373(5) Uani 1 1 d .
C11 C 0.33778(11) 0.44361(17) 0.32546(10) 0.0337(5) Uani 1 1 d .
C12 C 0.40095(10) 0.50449(16) 0.32161(9) 0.0309(4) Uani 1 1 d .
C13 C 0.43448(10) 0.48644(17) 0.27520(9) 0.0308(4) Uani 1 1 d .
C14 C 0.48027(10) 0.58238(16) 0.27305(9) 0.0290(4) Uani 1 1 d .
C15 C 0.49869(11) 0.79176(18) 0.43123(10) 0.0378(5) Uani 1 1 d .
C16 C 0.57618(12) 0.8266(2) 0.44435(11) 0.0526(6) Uani 1 1 d .
H16A H 0.5776 0.8519 0.3997 0.079 Uiso 1 1 calc R
H16B H 0.6072 0.7561 0.4632 0.079 Uiso 1 1 calc R
H16C H 0.5924 0.8937 0.4784 0.079 Uiso 1 1 calc R
C17 C 0.44957(12) 0.90499(19) 0.40752(11) 0.0484(6) Uani 1 1 d .
H17A H 0.4468 0.9335 0.3617 0.073 Uiso 1 1 calc R
H17B H 0.4689 0.9698 0.4427 0.073 Uiso 1 1 calc R
H17C H 0.4021 0.8831 0.4032 0.073 Uiso 1 1 calc R
C18 C 0.50439(15) 0.7535(2) 0.50530(11) 0.0563(7) Uani 1 1 d .
H18A H 0.5328 0.8135 0.5405 0.084 Uiso 1 1 calc R
H18B H 0.5271 0.6735 0.5175 0.084 Uiso 1 1 calc R
H18C H 0.4569 0.7494 0.5048 0.084 Uiso 1 1 calc R
C19 C 0.26120(10) 0.38954(18) 0.19577(10) 0.0371(5) Uani 1 1 d .
C20 C 0.24565(11) 0.28624(19) 0.15233(11) 0.0436(5) Uani 1 1 d .
H20 H 0.2477 0.2078 0.1723 0.052 Uiso 1 1 calc R
C21 C 0.22722(11) 0.2983(2) 0.07991(12) 0.0492(6) Uani 1 1 d .
H21 H 0.2182 0.2276 0.0512 0.059 Uiso 1 1 calc R
C22 C 0.22186(12) 0.4123(2) 0.04943(11) 0.0511(6) Uani 1 1 d .
H22 H 0.2086 0.4197 0.0000 0.061 Uiso 1 1 calc R
C23 C 0.23596(12) 0.5151(2) 0.09146(11) 0.0518(6) Uani 1 1 d .
H23 H 0.2318 0.5933 0.0707 0.062 Uiso 1 1 calc R
C24 C 0.25624(11) 0.50423(19) 0.16430(11) 0.0431(5) Uani 1 1 d .
H24 H 0.2668 0.5752 0.1929 0.052 Uiso 1 1 calc R
C25 C 0.42102(10) 0.37359(16) 0.23129(9) 0.0301(4) Uani 1 1 d .
C26 C 0.42152(10) 0.25982(17) 0.26249(10) 0.0369(5) Uani 1 1 d .
H26 H 0.4298 0.2561 0.3110 0.044 Uiso 1 1 calc R
C27 C 0.41005(11) 0.15221(19) 0.22363(11) 0.0457(5) Uani 1 1 d .
H27 H 0.4103 0.0763 0.2456 0.055 Uiso 1 1 calc R
C28 C 0.39827(11) 0.1563(2) 0.15286(12) 0.0495(6) Uani 1 1 d .
H28 H 0.3909 0.0833 0.1263 0.059 Uiso 1 1 calc R
C29 C 0.39729(11) 0.2679(2) 0.12086(11) 0.0459(6) Uani 1 1 d .
H29 H 0.3892 0.2705 0.0724 0.055 Uiso 1 1 calc R
C30 C 0.40798(10) 0.37581(19) 0.15908(9) 0.0361(5) Uani 1 1 d .
H30 H 0.4065 0.4514 0.1363 0.043 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'
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
C1 C1 C2 121.66(11) 2_655 .
C14 C2 C1 115.99(15) . .
C14 C2 C3 119.99(17) . .
C1 C2 C3 123.65(17) . .
C4 C3 C2 114.83(16) . .
C4 C3 C15 125.27(16) . .
C2 C3 C15 119.86(17) . .
C3 C4 C12 121.20(16) . .
C3 C4 C5 131.11(16) . .
C12 C4 C5 107.45(16) . .
C6 C5 C4 103.56(15) . .
C7 C6 C11 120.6(2) . .
C7 C6 C5 128.27(18) . .
C11 C6 C5 110.84(17) . .
C8 C7 C6 118.7(2) . .
C9 C8 C7 120.7(2) . .
C8 C9 C10 121.6(2) . .
C9 C10 C11 117.21(18) . .
C9 C10 C19 118.33(19) . .
C11 C10 C19 123.53(18) . .
C6 C11 C10 120.32(18) . .
C6 C11 C12 107.34(17) . .
C10 C11 C12 131.73(17) . .
C13 C12 C4 120.77(17) . .
C13 C12 C11 131.03(17) . .
C4 C12 C11 108.18(15) . .
C12 C13 C14 115.77(16) . .
C12 C13 C25 120.68(16) . .
C14 C13 C25 123.55(15) . .
C13 C14 C2 119.53(15) . .
C13 C14 C14 124.36(12) . 2_655
C2 C14 C14 115.88(12) . 2_655
C18 C15 C3 113.28(16) . .
C18 C15 C17 107.73(17) . .
C3 C15 C17 110.36(16) . .
C18 C15 C16 103.83(17) . .
C3 C15 C16 110.89(16) . .
C17 C15 C16 110.54(18) . .
C20 C19 C24 118.36(18) . .
C20 C19 C10 123.44(19) . .
C24 C19 C10 118.08(18) . .
C21 C20 C19 120.2(2) . .
C22 C21 C20 120.7(2) . .
C23 C22 C21 119.6(2) . .
C22 C23 C24 120.2(2) . .
C23 C24 C19 120.8(2) . .
C26 C25 C30 117.81(17) . .
C26 C25 C13 119.56(15) . .
C30 C25 C13 122.63(17) . .
C27 C26 C25 121.40(18) . .
C28 C27 C26 119.9(2) . .
C27 C28 C29 119.7(2) . .
C28 C29 C30 120.80(19) . .
C29 C30 C25 120.42(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C1 1.339(4) 2_655
C1 C2 1.436(2) .
C2 C14 1.420(2) .
C2 C3 1.440(2) .
C3 C4 1.384(3) .
C3 C15 1.538(3) .
C4 C12 1.421(2) .
C4 C5 1.526(2) .
C5 C6 1.492(3) .
C6 C7 1.392(3) .
C6 C11 1.395(2) .
C7 C8 1.381(3) .
C8 C9 1.379(3) .
C9 C10 1.400(3) .
C10 C11 1.402(3) .
C10 C19 1.484(3) .
C11 C12 1.485(3) .
C12 C13 1.398(2) .
C13 C14 1.417(2) .
C13 C25 1.481(2) .
C14 C14 1.476(3) 2_655
C15 C18 1.534(3) .
C15 C17 1.538(3) .
C15 C16 1.545(3) .
C19 C20 1.388(3) .
C19 C24 1.390(3) .
C20 C21 1.381(3) .
C21 C22 1.373(3) .
C22 C23 1.370(3) .
C23 C24 1.382(3) .
C25 C26 1.392(2) .
C25 C30 1.394(2) .
C26 C27 1.382(3) .
C27 C28 1.372(3) .
C28 C29 1.377(3) .
C29 C30 1.379(3) .
