Designing Hydrogen Bonds with Temperature-Dependent Proton Disorder: The Effect of Crystal Environment
Parkin, Andrew; Seaton, Colin C.; Blagden, Nicholas; Wilson, Chick C.; Crystal Growth & Design 7 (2007) 531–; doi:10.1021/cg060777p

data_4511317
_publ_section_title
;
 Designing Hydrogen Bonds with Temperature-Dependent Proton
 Disorder:&#x00A0; The Effect of Crystal Environment
;
_journal_issue                   3
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              531
_journal_paper_doi               10.1021/cg060777p
_journal_volume                  7
_journal_year                    2007
_chemical_formula_moiety         'C16 H15 N3 O8'
_chemical_formula_sum            'C16 H15 N3 O8'
_chemical_formula_weight         377.32
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-11-01
_audit_creation_method           CRYSTALS_ver_12.83
_cell_angle_alpha                90
_cell_angle_beta                 99.721(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.473(6)
_cell_length_b                   6.872(2)
_cell_length_c                   16.755(7)
_cell_measurement_reflns_used    11248
_cell_measurement_temperature    160
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     1642.5(11)
_computing_cell_refinement       'FSProcess in CrystalClear 1.3.6'
_computing_data_collection       'CrystalClear 1.3.6'
_computing_data_reduction        'FSProcess in CrystalClear 1.3.6'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      160
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Rigaku R-AXIS RAPID Image Plate Area Detector Diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15928
_diffrn_reflns_theta_full        27.474
_diffrn_reflns_theta_max         27.474
_diffrn_reflns_theta_min         3.052
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'FSProcess in CrystalClear 1.3.6'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       block
_exptl_crystal_F_000             784.040
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.51
_refine_ls_extinction_coef       39(15)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.8367
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3748
_refine_ls_number_restraints     67
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.001646
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1234
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1234
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                2048
_reflns_number_total             3698
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          1.538(11)
_oxford_structure_analysis_title 4daba_35dnba_complex_160k
_cod_data_source_file            4daba_35dnba_complex.cif
_cod_data_source_block           4daba_35dnba_complex_160k
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4511317