Crystal structure of 3-(methoxycarbonyl)-7-oxabicyclo[2.2.1]heptane-2-carboxylic acid, C9H12O5
Hou, Xuehui; Wang, Qinglong; Wang, Jianling; Li, Aiqin; Ding, Degang; Lv, Quanjian; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 651–652; doi:10.1515/ncrs-2021-0027

data_8104791
_publ_section_title
;
 Crystal structure of
 3-(methoxycarbonyl)-7-oxabicyclo[2.2.1]heptane-2-carboxylic acid, C9H12O5
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              651
_journal_page_last               652
_journal_paper_doi               10.1515/ncrs-2021-0027
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C9 H12 O5'
_chemical_formula_sum            'C9 H12 O5'
_chemical_formula_weight         200.19
_chemical_name_systematic
;
(1R,2R,3S,4R)-3-(methoxycarbonyl)-7-oxabicyclo[2.2.1]heptane-2-carboxylic 
acid, C9H12O5, C~9~H~12~O~5~
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_cell_angle_alpha                102.238(8)
_cell_angle_beta                 95.381(8)
_cell_angle_gamma                90.940(9)
_cell_formula_units_Z            2
_cell_length_a                   5.6537(6)
_cell_length_b                   7.7954(8)
_cell_length_c                   10.6841(9)
_cell_measurement_reflns_used    2097
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.9810
_cell_measurement_theta_min      4.2340
_cell_volume                     457.83(8)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)[2]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)[2]'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)[3]'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)[4]'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0832364000
_diffrn_orient_matrix_UB_12      0.0650857000
_diffrn_orient_matrix_UB_13      -0.1227964000
_diffrn_orient_matrix_UB_21      -0.0506090000
_diffrn_orient_matrix_UB_22      0.1802607000
_diffrn_orient_matrix_UB_23      0.0827522000
_diffrn_orient_matrix_UB_31      0.2559463000
_diffrn_orient_matrix_UB_32      0.0649275000
_diffrn_orient_matrix_UB_33      -0.0077508000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3149
_diffrn_reflns_theta_full        67.073
_diffrn_reflns_theta_max         67.073
_diffrn_reflns_theta_min         4.255
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.021
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)[1]
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_description       block
_exptl_crystal_F_000             212
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         3149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0673
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1345P)^2^+0.1742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2187
_refine_ls_wR_factor_ref         0.2279
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2411
_reflns_number_total             3149
_cod_data_source_file            suppl_j_ncrs-2021-0027_suppl.cif
_cod_data_source_block           exp_1115
_cod_database_code               8104791