#------------------------------------------------------------------------------
#$Date: 2017-10-13 07:28:26 +0200 (vie 13 de oct de 2017) $
#$Revision: 201972 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/37/2103791.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2103791
loop_
_publ_author_name
'Clemente, Dore Augusto'
'Marzotto, Armando'
_publ_section_title
;
 22 Space-group changes
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              43
_journal_page_last               50
_journal_paper_doi               10.1107/S0108768102022668
_journal_volume                  59
_journal_year                    2003
_chemical_formula_sum            'C15 Br O2'
_chemical_formula_weight         292.06
_chemical_name_common            Aplysinol
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           78
_symmetry_space_group_name_Hall  'P 4cw'
_symmetry_space_group_name_H-M   'P 43'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.750(5)
_cell_length_b                   13.750(5)
_cell_length_c                   7.319(4)
_cell_measurement_temperature    293(2)
_cell_volume                     1383.7(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.397
_diffrn_measured_fraction_theta_max 0.397
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0833
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            20164
_diffrn_reflns_theta_full        47.08
_diffrn_reflns_theta_max         47.08
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    2.959
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             564
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.407
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.015(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.308
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         5044
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.308
_refine_ls_R_factor_all          0.0093
_refine_ls_R_factor_gt           0.0085
_refine_ls_shift/su_max          0.261
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0466
_refine_ls_wR_factor_ref         0.0500
_reflns_number_gt                4914
_reflns_number_total             5044
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            an0613.cif
_cod_data_source_block           aplsol
_cod_original_sg_symbol_H-M      P43
_cod_database_code               2103791
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x, z+3/4'
'y, -x, z+1/4'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_type_symbol
Br1 0.889000(6) 0.835000(6) 0.499500(15) 0.02000(2) Uiso d 1 Br
O4 0.78510(5) 0.53550(5) -0.05260(9) 0.02000(10) Uiso d 1 O
O11 0.59220(5) 0.45900(5) 0.01880(9) 0.02000(10) Uiso d 1 O
C1 0.87600(6) 0.41500(7) 0.32000(11) 0.02000(12) Uiso d 1 C
C2 0.93450(7) 0.39800(7) 0.14500(11) 0.02000(12) Uiso d 1 C
C3 0.85700(6) 0.37750(6) 0.00900(12) 0.02000(12) Uiso d 1 C
C13 0.77000(7) 0.44650(7) 0.04250(10) 0.02000(13) Uiso d 1 C
C4 0.81100(7) 0.60800(7) 0.05750(11) 0.02000(12) Uiso d 1 C
C5 0.83300(6) 0.70200(6) 0.00850(12) 0.02000(12) Uiso d 1 C
C6 0.85750(7) 0.77150(7) 0.13450(11) 0.02000(12) Uiso d 1 C
C7 0.85500(7) 0.74450(6) 0.31800(11) 0.02000(12) Uiso d 1 C
C8 0.83200(7) 0.64800(7) 0.37700(11) 0.02000(12) Uiso d 1 C
C18 0.80750(6) 0.58100(6) 0.25200(12) 0.02000(11) Uiso d 1 C
C28 0.78500(6) 0.47400(6) 0.26400(11) 0.02000(12) Uiso d 1 C
C9 0.89200(7) 0.38000(7) -0.19600(11) 0.02000(12) Uiso d 1 C
C10 0.67600(6) 0.40250(7) -0.00650(12) 0.02000(12) Uiso d 1 C
C12 0.87550(7) 0.87700(7) 0.08550(11) 0.02000(12) Uiso d 1 C
C31 0.70000(7) 0.45700(7) 0.38600(11) 0.02000(13) Uiso d 1 C
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.2901 2.4595 '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'
C C 0.0033 0.0016 '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
C4 O4 C13 112.78(8)
C2 C1 C28 106.47(7)
C3 C2 C1 102.29(8)
C2 C3 C13 109.41(7)
C2 C3 C9 114.51(8)
C13 C3 C9 111.95(7)
O4 C13 C10 111.25(7)
O4 C13 C3 109.71(7)
C10 C13 C3 112.87(7)
O4 C13 C28 105.12(7)
C10 C13 C28 115.86(7)
C3 C13 C28 101.33(7)
O4 C4 C5 127.25(8)
O4 C4 C18 112.83(8)
C5 C4 C18 119.77(8)
C6 C5 C4 122.29(8)
C5 C6 C7 117.18(9)
C5 C6 C12 123.29(8)
C7 C6 C12 119.16(8)
C6 C7 C8 122.91(8)
C6 C7 Br1 119.91(7)
C8 C7 Br1 117.11(7)
C18 C8 C7 119.12(8)
C8 C18 C4 118.57(8)
C8 C18 C28 133.06(8)
C4 C18 C28 108.03(7)
C31 C28 C18 110.46(7)
C31 C28 C1 113.19(7)
C18 C28 C1 111.21(7)
C31 C28 C13 116.59(8)
C18 C28 C13 100.90(7)
C1 C28 C13 103.73(7)
O11 C10 C13 117.51(8)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Br1 C7 1.8793(11)
O4 C4 1.3304(12)
O4 C13 1.4231(12)
O11 C10 1.4020(11)
C1 C2 1.5304(13)
C1 C28 1.5465(13)
C2 C3 1.4852(13)
C3 C13 1.5464(14)
C3 C9 1.5761(14)
C13 C10 1.4715(14)
C13 C28 1.6774(14)
C4 C5 1.3750(13)
C4 C18 1.4719(14)
C5 C6 1.3701(13)
C6 C7 1.3938(14)
C6 C12 1.5147(13)
C7 C8 1.4308(13)
C8 C18 1.3413(13)
C18 C28 1.5060(13)
C28 C31 1.4893(13)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 4957886
