Kemp's acid at 120K
Alan Hazell; Hans Toftlund; Acta Crystallographica Section C 55 (1999) IUC9900079–; doi:10.1107/S0108270199098959

data_2008846
_publ_section_title
;
 Kemp's acid at 120K
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9900079
_journal_paper_doi               10.1107/S0108270199098959
_journal_volume                  55
_journal_year                    1999
_chemical_formula_sum            'C12 H18 O6'
_chemical_formula_weight         258.280
_chemical_name_common            'Kemp's acid'
_chemical_name_systematic
;
cis,cis-1,3,5-trimethylcyclohexane-1,3,5-tricarboxylic acid
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90
_cell_angle_beta                 101.5270(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3947(4)
_cell_length_b                   12.0150(5)
_cell_length_c                   12.8347(6)
_cell_measurement_reflns_used    6229
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.9
_cell_measurement_theta_min      2.3
_cell_volume                     1268.43(10)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_publication_material  KRYSTAL
_computing_structure_refinement
'modified ORFLS (Busing et al., 1962) and KRYSTAL'
_computing_structure_solution
'SIR97 (Cascarano et al., 1996) and KRYSTAL (Hazell, 1995)'
_diffrn_ambient_temperature      120
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method
;
\w rotation scans with narrow
frames
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'x-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.020
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10860
_diffrn_reflns_reduction_process 10860
_diffrn_reflns_theta_max         29.9
_diffrn_reflns_theta_min         2.3
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'multi-scan (SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.38(4)
_refine_diff_density_min         -0.19(4)
_refine_ls_extinction_coef       49(16)
_refine_ls_extinction_method
;
B-C type 1 Lorentzian isotropic
Becker & Coppens (1974)
;
_refine_ls_goodness_of_fit_ref   1.505
_refine_ls_hydrogen_treatment    refxyzu
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     236
_refine_ls_number_reflns         2709
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.031
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.00006
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.040
_reflns_number_gt                2709
_reflns_number_total             3512
_reflns_observed_criterion       I>3\s(I)
_cod_data_source_file            qb0103.cif
_cod_data_source_block           IUC9900079
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_site_thermal_displace_type' tag value 'Uij' was replaced with
'Uani' value 18 times.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '
w = 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^' was changed to 'calc'.
New tag '_refine_ls_weighting_details' was created. The value of the
new tag was set to 'w = 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1268.40(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2008846