Synthesis and structure of strained polycyclic cyclobutane-containing derivatives
Ianelli, S.; Nardelli, M.; Belletti, D.; Jamart-Grégoire, B.; Brosse, N.; Caubère, P.; Acta Crystallographica Section C 49 (1993) 1388–1392; doi:10.1107/S0108270193000319

data_2001549
_publ_section_title
;
 Synthesis and structure of strained polycyclic cyclobutane-containing
 derivatives
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1388
_journal_page_last               1392
_journal_paper_doi               10.1107/S0108270193000319
_journal_volume                  49
_journal_year                    1993
_chemical_formula_analytical     ' C12 H20 O3         '
_chemical_formula_sum            'C12 H20 O3'
_chemical_formula_weight         212.29
_chemical_name_systematic
;
Cis,anti,cis-8-methoxytricyclo[6.3.0.0^2,7^]undecan-2,3-diol
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_type_scat_source
'IntTabIV Tables 2.2A, 2.3.1 (O, C) and 2.2C (H)'
_cell_angle_alpha                90.00000
_cell_angle_beta                 105.550(10)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            2
_cell_length_a                   8.5730(10)
_cell_length_b                   10.6280(10)
_cell_length_c                   6.5440(10)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      25
_cell_volume                     574.42(13)
_computing_cell_refinement       LQPARM
_computing_molecular_graphics    ORTEP
_computing_publication_material  PARST
_computing_structure_refinement  'SHELX76 and SHELXL92'
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens-AED diffractometer'
_diffrn_measurement_method       '\q-2\q scan'
_diffrn_radiation_monochromator  'Ni filter'
_diffrn_radiation_source         'standard Cu anode'
_diffrn_radiation_type           'Cu K\a~1~'
_diffrn_radiation_wavelength     1.5405620
_diffrn_reflns_av_R_equivalents  0.0086
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1242
_diffrn_reflns_reduction_process
;
Standard. Lp correction.
;
_diffrn_reflns_theta_max         69.96
_diffrn_reflns_theta_min         5.36
_diffrn_standards_decay_%        'within statistical fluctuation'
_diffrn_standards_interval_count 50
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    .662
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_description
;
small prisms
;
_exptl_crystal_F_000             232
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.36
_refine_diff_density_min         -0.31
_refine_ls_extinction_coef       0.035(4)
_refine_ls_extinction_method
' F~c~^*^ = kF~c~[1+0.001F~c~^2^l^3^/sin(2q)]^-1/4^'
_refine_ls_goodness_of_fit_all   0.944
_refine_ls_goodness_of_fit_obs   1.049
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         1147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_restrained_S_obs      1.049
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_obs          0.0486
_refine_ls_shift/esd_max         -0.020
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^)+(0.0830P)^2^+0.0000P] where
P = (F~o~^2^+2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1384
_refine_ls_wR_factor_obs         0.1219
_reflns_number_observed          864
_reflns_number_total             1152
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ha1032.cif
_cod_data_source_block           4
_cod_original_cell_volume        574.40(10)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2001549