Crystal structures of two bicyclo[5.1.0]octanes: potassium <i>trans</i>-bicyclo[5.1.0]octane-4-carboxylate monohydrate and <i>cis</i>-bicyclo[5.1.0]octan-4-yl 4-bromobenzenesulfonate
Corfield, Peter W. R.; Kershaw, Richard A.; Acta Crystallographica Section E 73 (2017) 1357–1362; doi:10.1107/S2056989017011756

data_2242287
_publ_section_title
;
 Crystal structures of two bicyclo[5.1.0]octanes: potassium
 <i>trans</i>-bicyclo[5.1.0]octane-4-carboxylate monohydrate and
 <i>cis</i>-bicyclo[5.1.0]octan-4-yl 4-bromobenzenesulfonate
;
_journal_coeditor_code           PK2603
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1357
_journal_page_last               1362
_journal_paper_doi               10.1107/S2056989017011756
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'K +, C9 H13 O2 -, H2 O'
_chemical_formula_moiety         'K +, C9 H13 O2 -, H2 O'
_chemical_formula_sum            'C9 H15 K O3'
_chemical_formula_weight         210.31
_chemical_name_systematic
;
Potassium <i>trans</i>-bicyclo[5.1.0]octane-4-carboxylate monohydrate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   vecmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.148(13)
_cell_length_b                   8.631(9)
_cell_length_c                   7.674(10)
_cell_measurement_reflns_used    19
_cell_measurement_temperature    297(2)
_cell_volume                     1070(2)
_computing_cell_refinement
;
Corfield (1972)
;
_computing_data_collection
;
Corfield (1972)
;
_computing_data_reduction
;
Data reduction followed procedures in Corfield <i>et al.</i> (1973),
with <i>p</i> = 0.05
;
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
local superposition program (Corfield, 1972)
;
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Picker four-circle'
_diffrn_measurement_method       '\q/2\q scans'
_diffrn_radiation_monochromator  'oriented graphite 200 reflection'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.02
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1926
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         31.49
_diffrn_reflns_theta_min         1.261
_diffrn_standards_decay_%        -3.0(8)
_diffrn_standards_interval_count 220
_diffrn_standards_number         9
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
Busing & Levy (1957)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_meas      1.345(11)
_exptl_crystal_density_method
;
Flotation in benzene--carbon tetrachloride mixtures
;
_exptl_crystal_description       plate
_exptl_crystal_F_000             448
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .4
_exptl_crystal_size_min          .1
_refine_diff_density_max         0.153
_refine_diff_density_min         -0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1104
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+0.2500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0960
_reflns_number_gt                795
_reflns_number_total             1104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2603sup1.cif
_cod_data_source_block           I
_cod_database_code               2242287
_shelx_hkl_checksum              1020
_shelx_res_checksum              43713