<i>endo</i>-(1'<i>R</i>,2'<i>R</i>,5'<i>S</i>,7'<i>R</i>,9'<i>S</i>)-2-(9'-Benzyloxy-2'-phenyl-3',6'-dioxabicyclo[3.2.2]nonan-7'-yl)-7-bromo-5,8-dimethoxynaphthalen-1-yl acetate
Timothy J. Brenstrum; Margaret A. Brimble; Peter Turner; Acta Crystallographica Section E 57 (2001) o28–o29; doi:10.1107/S1600536800018092

data_2200073
_publ_section_title
;<i>endo</i>-(1'<i>R</i>,2'<i>R</i>,5'<i>S</i>,7'<i>R</i>,9'<i>S</i>)-2-(9'-Benzyloxy-2'-phenyl-3',6'-dioxabicyclo[3.2.2]nonan-7'-yl)-7-bromo-5,8-dimethoxynaphthalen-1-yl
 acetate
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o28
_journal_page_last               o29
_journal_paper_doi               10.1107/S1600536800018092
_journal_volume                  57
_journal_year                    2001
_chemical_formula_moiety         'C34 H33 Br O7'
_chemical_formula_sum            'C34 H33 Br O7'
_chemical_formula_weight         633.51
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   19.5150(10)
_cell_length_b                   23.667(2)
_cell_length_c                   6.541(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      30.2
_cell_measurement_theta_min      26.6
_cell_volume                     3021.0(10)
_computing_cell_refinement       'MSC AFC Diffractometer Control (MSC, 1995)'
_computing_data_collection       'MSC AFC Diffractometer Control (MSC, 1995)'
_computing_data_reduction        'teXsan (MSC, 1992)'
_computing_molecular_graphics    'teXsan for Windows (MSC, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, et. al. 1993)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  .0000
_diffrn_reflns_av_sigmaI/netI    .0395
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2962
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         65.0
_diffrn_reflns_theta_min         2.93
_diffrn_standards_decay_%        2.42
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.252
_exptl_absorpt_correction_T_max  .835
_exptl_absorpt_correction_T_min  .715
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       acicular
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          .55
_exptl_crystal_size_mid          .13
_exptl_crystal_size_min          .08
_refine_diff_density_max         .307
_refine_diff_density_min         -.340
_refine_ls_abs_structure_details
;
Flack (1983) and Bernardinelli & Flack(1985); No Friedel pairs
;
_refine_ls_abs_structure_Flack   -.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         2962
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          .0703
_refine_ls_R_factor_gt           .0356
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+0.6329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1139
_reflns_number_gt                2068
_reflns_number_total             2962
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               2200073