Solid-State Synthesis of New Diimide Compounds: A Two-Step Reaction Followed by X-ray Powder Diffraction
Neels, Antonia; Mantero, Déborah González; Stoeckli-Evans, Helen; Crystal Growth & Design 8 (2008) 1147–; doi:10.1021/cg070058q

data_4503052
_publ_section_title
;
 Solid-State Synthesis of New Diimide Compounds: A Two-Step Reaction
 Followed by X-ray Powder Diffraction
;
_journal_issue                   4
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1147
_journal_paper_doi               10.1021/cg070058q
_journal_volume                  8
_journal_year                    2008
_chemical_compound_source        synthesis
_chemical_formula_analytical     'C20 H16 N4 O8 Cl2'
_chemical_formula_moiety         'C10 H4 O8, 2(C5 H6 N2 Cl)'
_chemical_formula_structural     'C20 H16 N4 O8 Cl2'
_chemical_formula_sum            'C20 H16 Cl2 N4 O8'
_chemical_formula_weight         511.28
_chemical_name_systematic        ' ?'
_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'
_audit_creation_date             2005-05-25T11:12
_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_update_record
' 2005-05-25T11:12  Initial CIF as created by GSAS2CIF'
_cell_angle_alpha                90.0
_cell_angle_beta                 98.094(5)
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   22.3839(12)
_cell_length_b                   3.95869(15)
_cell_length_c                   11.6243(7)
_cell_measurement_temperature    293
_cell_volume                     1019.78(9)
_computing_data_collection       'WinXPow, Stoe & Cie (1997)'
_computing_data_reduction        'WinXPow, Stoe & Cie (1997)'
_computing_molecular_graphics    PLATON04
_computing_publication_material  GSAS
_computing_structure_refinement  GSAS
_computing_structure_solution    DASH
_diffrn_ambient_temperature      293
_diffrn_detector                 'linear PSD'
_diffrn_measurement_device_type  'Stoe STADIP'
_diffrn_radiation_monochromator  'curved Ge111'
_diffrn_radiation_polarisn_ratio 0.587
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a1'
_diffrn_source                   X-rays
_diffrn_source_target            Cu\Ka
_diffrn_source_type              'sealed tube'
_exptl_absorpt_coefficient_mu    3.415
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_process_details
;   GSAS Absorption/surface roughness correction: function number 0
 No correction is applied.
;
_exptl_crystal_density_diffrn    1.665
_pd_block_id                     2005-05-25T11:12|3a|g|g
_pd_calc_method                  'Rietveld Refinement'
_pd_char_colour                  white
_pd_char_particle_morphology     powder
_pd_instr_location               ' ?'
_pd_meas_2theta_range_inc        0.01
_pd_meas_2theta_range_max        99.99
_pd_meas_2theta_range_min        4.0
_pd_meas_number_of_points        9600
_pd_meas_scan_method             step
_pd_phase_name                   3a
_pd_prep_temperature             293
_pd_proc_2theta_range_inc        0.01
_pd_proc_2theta_range_max        99.96977
_pd_proc_2theta_range_min        3.97977
_pd_proc_info_datetime           2005-05-25T11:12:49
_pd_proc_info_excluded_regions
; data <6deg excluded - no reflections observed
data >80deg excluded - strong overlapp of reflections
;
_pd_proc_ls_background_function
;   GSAS Background function number 2 with 12 terms.
 Cosine Fourier series
      1:    105968.     2:   -156746.     3:    29880.8     4:    99571.0    
      5:   -171864.     6:    175323.     7:   -134856.     8:    83297.7    
      9:   -42059.2    10:    16699.0    11:   -4849.74    12:    766.084    
;
_pd_proc_ls_peak_cutoff          0.00100
_pd_proc_ls_pref_orient_corr
;   March-Dollase
 AXIS  1 Ratio=     1.013 Frac     1.000  h= 2.000  k= 0.000  l= 0.000
 AXIS  2 Ratio=     1.000 Frac     0.000  h= 0.000  k= 1.000  l= 1.000
 Prefered orientation correction range: Min=   0.96321, Max=   1.01892
;
_pd_proc_ls_profile_function
;
 CW Profile function number 2 with  18 terms
 Profile coefficients for Simpson's rule integration of pseudovoigt function
 C.J. Howard (1982). J. Appl. Cryst.,15,615-620.
 P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
 Peak tails are ignored  where the intensity is below 0.0010 times the peak
   Aniso. broadening axis   0.0   0.0   1.0
;
_pd_proc_ls_prof_R_factor        0.0563
_pd_proc_ls_prof_wR_expected     0.0274
_pd_proc_ls_prof_wR_factor       0.0781
_pd_proc_number_of_points        9600
_pd_spec_mounting
;
capillary
;
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_spec_size_axial              0.5
_pd_spec_size_equat              5
_pd_spec_size_thick              0.5
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.251
_refine_ls_goodness_of_fit_all   3.03
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_restraints     90
_refine_ls_R_Fsqd_factor         0.07870
_refine_ls_shift/su_max          0.02
_refine_ls_shift/su_mean         0.00
_reflns_d_resolution_high        1.200
_reflns_d_resolution_low         11.080
_reflns_limit_h_max              20
_reflns_limit_h_min              0
_reflns_limit_k_max              3
_reflns_limit_k_min              0
_reflns_limit_l_max              10
_reflns_limit_l_min              -10
_reflns_number_total             1238
_cod_data_source_file            cg070058q-file006.cif
_cod_data_source_block           3a_publ
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'N' changed to 'n' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (45
times).

'_geom_angle_publ_flag' value 'N' changed to 'n' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (41 time).

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_database_code               4503052
_refine_ls_r_f_factor            0.0504
_gsas_exptl_extinct_corr_t_min   1.00000
_gsas_exptl_extinct_corr_t_max   1.00000