#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:47:12 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180155 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/51/7105126.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_7105126
loop_
_publ_author_name
'Nicolaou, K C'
'Dong, Lin'
'Deng, Lujiang'
'Talbot, Adam C'
'Chen, David Y-K'
_publ_section_title
;
 Synthesis of functionalized maoecrystal V core structures.
;
_journal_issue                   1
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              70
_journal_page_last               72
_journal_paper_doi               10.1039/b917045f
_journal_volume                  46
_journal_year                    2009
_chemical_formula_moiety         'C16 H18 O4'
_chemical_formula_sum            'C16 H18 O4'
_chemical_formula_weight         274.30
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.25(3)
_cell_angle_beta                 98.41(3)
_cell_angle_gamma                104.21(3)
_cell_formula_units_Z            2
_cell_length_a                   6.7342(13)
_cell_length_b                   8.6721(17)
_cell_length_c                   11.458(2)
_cell_measurement_reflns_used    2498
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      30.9188
_cell_measurement_theta_min      1.8600
_cell_volume                     619.8(2)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'CCD area deterctor'
_diffrn_measurement_method       'ω scans'
_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  0.0147
_diffrn_reflns_av_sigmaI/netI    0.0125
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8536
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  0.9750
_exptl_absorpt_correction_T_min  0.9640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, R.H. (1995) Acta Cryst A51, 33-38'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             292
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2987
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0378
_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)+(0.0500P)²+0.2868P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.0997
_reflns_number_gt                2919
_reflns_number_total             2987
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b917045f.txt
_cod_data_source_block           15
_cod_database_code               7105126
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
O3 O 0.94309(11) 0.33020(9) 0.83046(7) 0.01362(16) Uani 1 1 d . . .
O2 O 1.16269(13) 0.46527(11) 0.62179(8) 0.02097(19) Uani 1 1 d . . .
O1 O 0.35923(13) 0.15064(10) 0.50115(7) 0.02170(19) Uani 1 1 d . . .
O4 O 0.67824(15) 0.77408(11) 0.98475(8) 0.0257(2) Uani 1 1 d . . .
C1 C 0.99954(16) 0.41154(12) 0.65099(9) 0.0136(2) Uani 1 1 d . . .
C2 C 0.68818(16) 0.57724(12) 0.65842(9) 0.0135(2) Uani 1 1 d . . .
H2A H 0.5444 0.5886 0.6489 0.016 Uiso 1 1 calc R . .
H2B H 0.7145 0.5373 0.5762 0.016 Uiso 1 1 calc R . .
C3 C 1.06851(16) 0.63094(12) 0.86137(9) 0.0142(2) Uani 1 1 d . . .
H3A H 1.2001 0.6738 0.8349 0.017 Uiso 1 1 calc R . .
H3B H 1.1047 0.6187 0.9452 0.017 Uiso 1 1 calc R . .
C4 C 0.62444(16) 0.50722(12) 0.84920(9) 0.0140(2) Uani 1 1 d . . .
H4A H 0.4722 0.4927 0.8260 0.017 Uiso 1 1 calc R . .
H4B H 0.6471 0.4400 0.9070 0.017 Uiso 1 1 calc R . .
C5 C 0.71064(15) 0.45319(12) 0.73531(9) 0.01120(19) Uani 1 1 d . . .
C6 C 0.62841(17) 0.11822(13) 0.84096(9) 0.0155(2) Uani 1 1 d . . .
H6A H 0.6064 0.2070 0.9034 0.019 Uiso 1 1 calc R . .
H6B H 0.7009 0.0530 0.8836 0.019 Uiso 1 1 calc R . .
C7 C 0.43066(16) 0.17345(12) 0.60924(10) 0.0145(2) Uani 1 1 d . . .
C8 C 0.65784(16) 0.26659(12) 0.66453(9) 0.0125(2) Uani 1 1 d . . .
C9 C 0.76288(16) 0.19307(12) 0.76073(9) 0.0142(2) Uani 1 1 d . . .
H9 H 0.8173 0.1055 0.7161 0.017 Uiso 1 1 calc R . .
C10 C 0.80637(16) 0.27670(12) 0.57368(9) 0.0148(2) Uani 1 1 d . . .
H10A H 0.8388 0.1710 0.5469 0.018 Uiso 1 1 calc R . .
H10B H 0.7460 0.3080 0.5012 0.018 Uiso 1 1 calc R . .
C11 C 0.93279(16) 0.75079(12) 0.85915(9) 0.0146(2) Uani 1 1 d . . .
H11 H 1.0144 0.8651 0.9072 0.018 Uiso 1 1 calc R . .
C12 C 0.30307(17) 0.10569(13) 0.69464(10) 0.0174(2) Uani 1 1 d . . .
H12A H 0.1645 0.0332 0.6472 0.021 Uiso 1 1 calc R . .
H12B H 0.2802 0.1975 0.7539 0.021 Uiso 1 1 calc R . .
C13 C 0.94323(15) 0.46641(12) 0.77535(9) 0.01146(19) Uani 1 1 d . . .
C14 C 0.74059(17) 0.68863(13) 0.90865(10) 0.0156(2) Uani 1 1 d . . .
C15 C 0.41695(17) 0.00737(13) 0.76392(10) 0.0173(2) Uani 1 1 d . . .
H15A H 0.3295 -0.0391 0.8175 0.021 Uiso 1 1 calc R . .
H15B H 0.4385 -0.0852 0.7047 0.021 Uiso 1 1 calc R . .
C16 C 0.84961(17) 0.74621(13) 0.72500(10) 0.0158(2) Uani 1 1 d . . .
H16A H 0.9679 0.7648 0.6826 0.019 Uiso 1 1 calc R . .
H16B H 0.7824 0.8354 0.7227 0.019 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'
O O 0.0106 0.0060 '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
C13 O3 C9 107.02(8) . . ?
O2 C1 C10 127.91(10) . . ?
O2 C1 C13 126.80(10) . . ?
C10 C1 C13 105.29(9) . . ?
C5 C2 C16 108.52(8) . . ?
C5 C2 H2A 110.0 . . ?
C16 C2 H2A 110.0 . . ?
C5 C2 H2B 110.0 . . ?
C16 C2 H2B 110.0 . . ?
H2A C2 H2B 108.4 . . ?
C13 C3 C11 107.86(8) . . ?
C13 C3 H3A 110.1 . . ?
C11 C3 H3A 110.1 . . ?
C13 C3 H3B 110.1 . . ?
C11 C3 H3B 110.1 . . ?
H3A C3 H3B 108.4 . . ?
C14 C4 C5 107.66(9) . . ?
C14 C4 H4A 110.2 . . ?
C5 C4 H4A 110.2 . . ?
C14 C4 H4B 110.2 . . ?
C5 C4 H4B 110.2 . . ?
H4A C4 H4B 108.5 . . ?
C4 C5 C13 108.77(8) . . ?
C4 C5 C2 105.70(8) . . ?
C13 C5 C2 109.62(8) . . ?
C4 C5 C8 121.77(8) . . ?
C13 C5 C8 92.26(8) . . ?
C2 C5 C8 117.33(8) . . ?
C9 C6 C15 110.29(9) . . ?
C9 C6 H6A 109.6 . . ?
C15 C6 H6A 109.6 . . ?
C9 C6 H6B 109.6 . . ?
C15 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
O1 C7 C12 122.72(10) . . ?
O1 C7 C8 121.10(10) . . ?
C12 C7 C8 116.13(9) . . ?
C7 C8 C10 115.78(9) . . ?
C7 C8 C9 113.83(9) . . ?
C10 C8 C9 103.71(8) . . ?
C7 C8 C5 117.94(9) . . ?
C10 C8 C5 101.22(8) . . ?
C9 C8 C5 102.31(8) . . ?
O3 C9 C6 112.84(9) . . ?
O3 C9 C8 103.15(8) . . ?
C6 C9 C8 117.45(9) . . ?
O3 C9 H9 107.6 . . ?
C6 C9 H9 107.6 . . ?
C8 C9 H9 107.6 . . ?
C1 C10 C8 101.68(8) . . ?
C1 C10 H10A 111.4 . . ?
C8 C10 H10A 111.4 . . ?
C1 C10 H10B 111.4 . . ?
C8 C10 H10B 111.4 . . ?
H10A C10 H10B 109.3 . . ?
C14 C11 C3 108.99(9) . . ?
C14 C11 C16 105.57(9) . . ?
C3 C11 C16 108.93(9) . . ?
C14 C11 H11 111.1 . . ?
C3 C11 H11 111.1 . . ?
C16 C11 H11 111.1 . . ?
C7 C12 C15 110.50(9) . . ?
C7 C12 H12A 109.6 . . ?
C15 C12 H12A 109.6 . . ?
C7 C12 H12B 109.6 . . ?
C15 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
O3 C13 C3 112.50(8) . . ?
O3 C13 C5 104.59(8) . . ?
C3 C13 C5 113.33(9) . . ?
O3 C13 C1 104.45(8) . . ?
C3 C13 C1 119.54(9) . . ?
C5 C13 C1 100.76(8) . . ?
O4 C14 C11 124.10(10) . . ?
O4 C14 C4 122.46(10) . . ?
C11 C14 C4 113.39(9) . . ?
C6 C15 C12 110.49(9) . . ?
C6 C15 H15A 109.6 . . ?
C12 C15 H15A 109.6 . . ?
C6 C15 H15B 109.6 . . ?
C12 C15 H15B 109.6 . . ?
H15A C15 H15B 108.1 . . ?
C11 C16 C2 110.39(9) . . ?
C11 C16 H16A 109.6 . . ?
C2 C16 H16A 109.6 . . ?
C11 C16 H16B 109.6 . . ?
C2 C16 H16B 109.6 . . ?
H16A C16 H16B 108.1 . . ?
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
O3 C13 1.4527(12) . ?
O3 C9 1.4595(14) . ?
O2 C1 1.2077(14) . ?
O1 C7 1.2163(14) . ?
O4 C14 1.2130(14) . ?
C1 C10 1.5234(16) . ?
C1 C13 1.5361(14) . ?
C2 C5 1.5489(14) . ?
C2 C16 1.5531(16) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C13 1.5126(15) . ?
C3 C11 1.5450(15) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C14 1.5284(15) . ?
C4 C5 1.5346(14) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C13 1.5350(14) . ?
C5 C8 1.5745(14) . ?
C6 C9 1.5147(15) . ?
C6 C15 1.5269(16) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C12 1.5111(15) . ?
C7 C8 1.5122(15) . ?
C8 C10 1.5466(14) . ?
C8 C9 1.5536(14) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C14 1.5131(15) . ?
C11 C16 1.5456(15) . ?
C11 H11 1.0000 . ?
C12 C15 1.5412(16) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
