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#$Date: 2016-03-26 16:27:48 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180340 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/09/7200991.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_7200991
loop_
_publ_author_name
'Salorinne, Kirsi'
'Nissinen, Maija'
_publ_section_title
;
 Twisting of the resorcinarene core due to solvent effects upon
 crystallization
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              1572
_journal_paper_doi               10.1039/b902718a
_journal_volume                  11
_journal_year                    2009
_chemical_formula_sum            'C46 H60 O10'
_chemical_formula_weight         772.94
_chemical_name_systematic
;
?
;
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4267(4)
_cell_length_b                   16.4267(4)
_cell_length_c                   16.1350(7)
_cell_measurement_temperature    173(2)
_cell_volume                     4353.8(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6315
_diffrn_reflns_theta_full        66.90
_diffrn_reflns_theta_max         66.90
_diffrn_reflns_theta_min         3.81
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_T_max  0.8788
_exptl_absorpt_correction_T_min  0.8788
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'Denzo (otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       0.0030(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1913
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0758
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1369P)²+1.9533P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2184
_refine_ls_wR_factor_ref         0.2285
_reflns_number_gt                1634
_reflns_number_total             1913
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b902718a.txt
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P4/ncc
_cod_database_code               7200991
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y, -x, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'
'-y-1/2, -x-1/2, z-1/2'
'y, x, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.42138(13) 0.14997(13) 0.53793(12) 0.0334(6) Uani 1 1 d . . .
C2 C 0.37458(13) 0.34608(13) 0.56802(12) 0.0326(6) Uani 1 1 d . . .
H2 H 0.3447 0.3229 0.6126 0.039 Uiso 1 1 calc R . .
C3 C 0.44067(13) 0.30245(14) 0.53662(13) 0.0341(6) Uani 1 1 d . . .
C4 C 0.48235(14) 0.33681(15) 0.46968(14) 0.0408(6) Uani 1 1 d . . .
C5 C 0.41207(16) 0.04022(15) 0.43782(15) 0.0437(7) Uani 1 1 d . . .
H5 H 0.4351 0.0105 0.3931 0.052 Uiso 1 1 calc R . .
C6 C 0.45354(14) 0.10582(15) 0.47114(14) 0.0384(6) Uani 1 1 d . . .
C7 C 0.46757(13) 0.22224(13) 0.57452(13) 0.0338(6) Uani 1 1 d . . .
H7 H 0.5259 0.2148 0.5587 0.041 Uiso 1 1 calc R . .
C29 C 0.46523(14) 0.22417(14) 0.67020(13) 0.0389(6) Uani 1 1 d . . .
H29A H 0.4933 0.2739 0.6900 0.047 Uiso 1 1 calc R . .
H29B H 0.4079 0.2270 0.6888 0.047 Uiso 1 1 calc R . .
C30 C 0.50509(19) 0.15054(17) 0.70853(16) 0.0567(8) Uani 1 1 d . . .
H30A H 0.4717 0.1022 0.6977 0.085 Uiso 1 1 calc R . .
H30B H 0.5102 0.1586 0.7685 0.085 Uiso 1 1 calc R . .
H30C H 0.5593 0.1429 0.6843 0.085 Uiso 1 1 calc R . .
C37 C 0.56042(18) 0.09091(18) 0.36987(17) 0.0582(8) Uani 1 1 d . . .
H37A H 0.5682 0.0331 0.3828 0.087 Uiso 1 1 calc R . .
H37B H 0.6129 0.1153 0.3552 0.087 Uiso 1 1 calc R . .
H37C H 0.5227 0.0963 0.3232 0.087 Uiso 1 1 calc R . .
O4 O 0.54807(12) 0.30051(13) 0.43231(12) 0.0574(7) Uani 1 1 d . . .
H4 H 0.546(2) 0.249(2) 0.445(2) 0.069 Uiso 1 1 d . . .
O6 O 0.52757(10) 0.13175(11) 0.44075(11) 0.0475(6) Uani 1 1 d . . .
C42 C 0.3151(6) 0.2111(7) 0.3540(4) 0.103(3) Uani 0.50 1 d P . .
H42A H 0.3551 0.1865 0.3165 0.155 Uiso 0.50 1 calc PR . .
H42B H 0.2916 0.1687 0.3894 0.155 Uiso 0.50 1 calc PR . .
H42C H 0.3420 0.2521 0.3886 0.155 Uiso 0.50 1 calc PR . .
C41 C 0.2500 0.2500 0.3050(3) 0.0411(11) Uani 1 4 d S . .
O40 O 0.2500 0.2500 0.23074(19) 0.0475(9) Uani 1 4 d S . .
O50 O 0.7500 0.2500 0.3793(15) 0.277(10) Uiso 0.50 2 d SP . .
C51 C 0.7500 0.2500 0.4618(10) 0.123(5) Uiso 0.50 2 d SP . .
C52 C 0.6859(12) 0.2158(12) 0.5174(12) 0.202(7) Uiso 0.50 1 d P . .
H52A H 0.6423 0.1920 0.4838 0.303 Uiso 0.50 1 calc PR . .
H52B H 0.6635 0.2594 0.5521 0.303 Uiso 0.50 1 calc PR . .
H52C H 0.7098 0.1737 0.5528 0.303 Uiso 0.50 1 calc PR . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 '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
_geom_angle_publ_flag
C2 C1 C6 117.0(2) 4 . ?
C2 C1 C7 122.21(18) 4 . ?
C6 C1 C7 120.8(2) . . ?
C1 C2 C3 123.80(19) 3 . ?
C2 C3 C4 117.0(2) . . ?
C2 C3 C7 121.71(19) . . ?
C4 C3 C7 121.3(2) . . ?
O4 C4 C5 115.7(2) . 3 ?
O4 C4 C3 123.3(2) . . ?
C5 C4 C3 121.0(2) 3 . ?
C6 C5 C4 120.2(2) . 4 ?
O6 C6 C5 122.5(2) . . ?
O6 C6 C1 116.5(2) . . ?
C5 C6 C1 121.1(2) . . ?
C3 C7 C1 111.97(17) . . ?
C3 C7 C29 112.18(17) . . ?
C1 C7 C29 112.95(18) . . ?
C30 C29 C7 112.50(19) . . ?
C6 O6 C37 118.15(19) . . ?
O40 C41 C42 122.4(4) . 3 ?
O40 C41 C42 122.4(4) . . ?
C42 C41 C42 73.3(3) 3 . ?
O40 C41 C42 122.4(4) . 4 ?
C42 C41 C42 115.3(7) 3 4 ?
C42 C41 C42 73.3(3) . 4 ?
O40 C41 C42 122.4(4) . 2 ?
C42 C41 C42 73.3(3) 3 2 ?
C42 C41 C42 115.3(7) . 2 ?
C42 C41 C42 73.3(3) 4 2 ?
C51 C51 C52 74.3(12) 11_666 11_666 ?
C51 C51 C52 74.3(12) 11_666 12_656 ?
C52 C51 C52 149(2) 11_666 12_656 ?
C51 C51 O50 180.000(6) 11_666 . ?
C52 C51 O50 105.7(12) 11_666 . ?
C52 C51 O50 105.7(12) 12_656 . ?
C51 C51 C52 53.1(9) 11_666 . ?
C52 C51 C52 80.7(8) 11_666 . ?
C52 C51 C52 80.7(8) 12_656 . ?
O50 C51 C52 126.9(9) . . ?
C51 C51 C52 53.1(9) 11_666 2_655 ?
C52 C51 C52 80.7(8) 11_666 2_655 ?
C52 C51 C52 80.7(8) 12_656 2_655 ?
O50 C51 C52 126.9(9) . 2_655 ?
C52 C51 C52 106.1(18) . 2_655 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.389(3) 4 ?
C1 C6 1.402(3) . ?
C1 C7 1.528(3) . ?
C2 C1 1.389(3) 3 ?
C2 C3 1.396(3) . ?
C3 C4 1.398(3) . ?
C3 C7 1.518(3) . ?
C4 O4 1.373(3) . ?
C4 C5 1.389(3) 3 ?
C5 C6 1.384(3) . ?
C5 C4 1.389(3) 4 ?
C6 O6 1.379(3) . ?
C7 C29 1.545(3) . ?
C29 C30 1.508(3) . ?
C37 O6 1.431(3) . ?
C42 C41 1.476(7) . ?
C41 O40 1.199(5) . ?
C41 C42 1.476(7) 3 ?
C41 C42 1.476(7) 4 ?
C41 C42 1.476(7) 2 ?
O50 C51 1.33(2) . ?
C51 C51 1.23(3) 11_666 ?
C51 C52 1.239(18) 11_666 ?
C51 C52 1.239(18) 12_656 ?
C51 C52 1.493(16) . ?
C51 C52 1.493(16) 2_655 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4 O6 0.87(4) 1.96(4) 2.796(3) 163(3) .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -1.7(3) 3 . . . ?
C1 C2 C3 C7 176.93(19) 3 . . . ?
C2 C3 C4 O4 -179.6(2) . . . . ?
C7 C3 C4 O4 1.8(4) . . . . ?
C2 C3 C4 C5 1.7(3) . . . 3 ?
C7 C3 C4 C5 -176.9(2) . . . 3 ?
C4 C5 C6 O6 -178.7(2) 4 . . . ?
C4 C5 C6 C1 0.8(4) 4 . . . ?
C2 C1 C6 O6 178.77(19) 4 . . . ?
C7 C1 C6 O6 -0.6(3) . . . . ?
C2 C1 C6 C5 -0.8(3) 4 . . . ?
C7 C1 C6 C5 179.9(2) . . . . ?
C2 C3 C7 C1 86.8(2) . . . . ?
C4 C3 C7 C1 -94.6(2) . . . . ?
C2 C3 C7 C29 -41.4(3) . . . . ?
C4 C3 C7 C29 137.1(2) . . . . ?
C2 C1 C7 C3 -85.2(2) 4 . . . ?
C6 C1 C7 C3 94.1(2) . . . . ?
C2 C1 C7 C29 42.6(3) 4 . . . ?
C6 C1 C7 C29 -138.1(2) . . . . ?
C3 C7 C29 C30 -170.2(2) . . . . ?
C1 C7 C29 C30 62.1(3) . . . . ?
C5 C6 O6 C37 2.7(4) . . . . ?
C1 C6 O6 C37 -176.8(2) . . . . ?
