The Anisotropic Compression of the Crystal Structure of 3-Aza-bicyclo(3.3.1)nonane-2,4-dione to 7.1 GPa
Wood, Peter A.; Haynes, Delia A.; Lennie, Alistair R.; Motherwell, W. D. Samuel; Parsons, Simon; Pidcock, Elna; Warren, John E.; Crystal Growth & Design 8 (2008) 549–; doi:10.1021/cg0705815

data_4503132
_publ_section_title
;
 The Anisotropic Compression of the Crystal Structure of
 3-Aza-bicyclo(3.3.1)nonane-2,4-dione to 7.1 GPa
;
_journal_issue                   2
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              549
_journal_paper_doi               10.1021/cg0705815
_journal_volume                  8
_journal_year                    2008
_chemical_compound_source        'Sigma Aldrich'
_chemical_formula_moiety         'C8 H11 N1 O2'
_chemical_formula_sum            'C8 H11 N O2'
_chemical_formula_weight         153.18
_chemical_name_systematic        3-aza-bicyclo(3.3.1)nonane-2,4-dione
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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             06-08-09
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 96.38(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.564(7)
_cell_length_b                   10.0876(18)
_cell_length_c                   7.6419(12)
_cell_measurement_reflns_used    483
_cell_measurement_temperature    298
_cell_measurement_theta_max      25
_cell_measurement_theta_min      4
_cell_volume                     656.1(6)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_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    'Model taken from ambient pressure structure'
_diffrn_ambient_pressure         1900000
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.326
_diffrn_measured_fraction_theta_max 0.305
_diffrn_measurement_device_type  'Bruker-Nonius ApexII CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8460
_diffrn_reflns_av_R_equivalents  0.067
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            1143
_diffrn_reflns_theta_full        25.048
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_min         3.998
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS version 2006/1'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       block
_exptl_crystal_F_000             328
_exptl_crystal_recrystallization_method
'Recrystallised by application of pressure from methanol/ethanol solution'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.15
_refine_diff_density_min         -0.14
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9392
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     45
_refine_ls_number_reflns         239
_refine_ls_number_restraints     29
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.000048
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 14.8 22.6 11.7 5.12 1.72 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1401
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1401
_reflns_limit_h_max              2
_reflns_limit_h_min              -3
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              7
_reflns_limit_l_min              0
_reflns_number_gt                203
_reflns_number_total             261
_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          0.687(10)
_cod_data_source_file            cg0705815-file001.cif
_cod_data_source_block           19kbar
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C8 H11 N1 O2'
_cod_database_code               4503132