Use of a CCD diffractometer in crystal structure determinations at high pressure
Dawson, Alice; Allan, David R.; Parsons, Simon; Ruf, Michael; Journal of Applied Crystallography 37 (2004) 410–416; doi:10.1107/S0021889804007149

data_2300042
_publ_section_title
;
 Use of a CCD diffractometer in crystal structure determinations at
 high pressure
;
_journal_issue                   3
_journal_name_full               'Journal of Applied Crystallography'
_journal_page_first              410
_journal_page_last               416
_journal_paper_doi               10.1107/S0021889804007149
_journal_volume                  37
_journal_year                    2004
_chemical_formula_moiety         ' C2 H4 O2 '
_chemical_formula_sum            'C2 H4 O2'
_chemical_formula_weight         60.05
_chemical_name_systematic
;
acetic 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_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           CRYSTALS_ver_12.20
_cell_angle_alpha                90
_cell_angle_beta                 93.177(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.9447(6)
_cell_length_b                   13.028(2)
_cell_length_c                   5.6407(9)
_cell_measurement_reflns_used    193
_cell_measurement_temperature    293
_cell_measurement_theta_max      20
_cell_measurement_theta_min      4
_cell_volume                     289.44(8)
_computing_cell_refinement
;
 SAINT (Siemens ,1995)
;
_computing_data_collection
;
 SMART (Siemens, 1993)
;
_computing_data_reduction
;
 SAINT (Siemens ,1995)
;
_computing_molecular_graphics
;
 XP
;
_computing_publication_material
;
 CRYSTALS (Watkin et al 2003)
;
_computing_structure_refinement
;
 CRYSTALS (Watkin et al 2003)
;
_computing_structure_solution
;
 SHELXS 86 (Sheldrick, 1986)
;
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.707
_diffrn_measured_fraction_theta_max 0.610
_diffrn_measurement_device_type
;
Bruker SMART
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2385
_diffrn_reflns_reduction_process
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        17.544
_diffrn_reflns_theta_max         23.084
_diffrn_reflns_theta_min         3.942
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.597
_exptl_absorpt_correction_type   'empirical, analytical and multi-scan'
_exptl_absorpt_process_details
;
 SHADE (Parsons, 2004)
 SADABS (Siemens, 1996)
 Data from Sadabs given below.
;
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             128
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.14
_refine_diff_density_min         -0.11
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0384
_refine_ls_hydrogen_treatment    'restrained refall'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     50
_refine_ls_number_reflns         249
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.000935
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method = SHELXL 97 (Sheldrick, 1997)
 W = 1. / [Sigma^2^(Fo^2^)+(0.0428p)^2^+ 0.0675p]
 where p=0.333*max(Fo^2^,0) + 0.667*Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0892
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0892
_reflns_number_gt                189
_reflns_number_total             251
_reflns_threshold_expression     I>2.00u(I)
_cod_data_source_file            he5280.cif
_cod_data_source_block           he5280
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        ' C2 H4 O2 '
_cod_database_code               2300042