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_4503050
_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     'C18 H16 N6 O8'
_chemical_formula_moiety         'C10 H4 O8, 2(C4 H6 N3)'
_chemical_formula_structural     'C18 H16 N6 O8'
_chemical_formula_sum            'C18 H16 N6 O8'
_chemical_formula_weight         444.36
_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'
_audit_creation_date             2005-12-02T12:17
_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_update_record
' 2005-12-02T12:17  Initial CIF as created by GSAS2CIF'
_cell_angle_alpha                90.0
_cell_angle_beta                 94.697(4)
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   11.2777(6)
_cell_length_b                   12.8578(5)
_cell_length_c                   6.47179(14)
_cell_measurement_temperature    293
_cell_volume                     935.30(7)
_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 0.604
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu Kalpha1'
_diffrn_radiation_wavelength     1.54051
_diffrn_source                   X-rays
_diffrn_source_target            Cu\Ka
_diffrn_source_type              'sealed tube'
_exptl_absorpt_coefficient_mu    1.09
_exptl_absorpt_correction_T_max  1.30730
_exptl_absorpt_correction_T_min  1.30024
_exptl_absorpt_process_details
;   GSAS Absorption/surface roughness correction: function number 0
 Debye-Scherrer absorption correction
Term (= MU.r/wave) =    -0.10000    
Correction is not refined.
;
_exptl_crystal_density_diffrn    1.578
_pd_block_id                     2005-12-02T12:17|1A-120|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        89.99
_pd_meas_2theta_range_min        4.0
_pd_meas_number_of_points        8600
_pd_meas_scan_method             step
_pd_phase_name                   1a-120
_pd_prep_temperature             293
_pd_proc_2theta_range_inc        0.01
_pd_proc_2theta_range_max        89.97548
_pd_proc_2theta_range_min        3.98548
_pd_proc_info_datetime           2005-12-02T12:17:20
_pd_proc_info_excluded_regions
; data <4deg excluded - no reflections observed
data >80deg excluded - strong overlapp of reflections
;
_pd_proc_ls_background_function
;   GSAS Background function number 2 with 24 terms.
 Cosine Fourier series
      1:   -767.151     2:    6093.85     3:   -6419.40     4:   -2262.71    
      5:    11174.2     6:   -4683.98     7:   -12041.5     8:    16283.1    
      9:   -1568.03    10:   -13183.8    11:    7400.96    12:    11908.4    
     13:   -22016.9    14:    14092.9    15:   -1973.27    16:    1687.36    
     17:   -12206.9    18:    20811.0    19:   -19553.4    20:    11491.2    
     21:   -3994.41    22:    332.861    23:    321.555    24:   -147.766    
;
_pd_proc_ls_peak_cutoff          0.00500
_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 0.0050 times the peak
   Aniso. broadening axis   0.0   0.0   1.0
;
_pd_proc_ls_prof_R_factor        0.0517
_pd_proc_ls_prof_wR_expected     0.0274
_pd_proc_ls_prof_wR_factor       0.0682
_pd_proc_number_of_points        8600
_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         0.188
_refine_diff_density_min         -0.232
_refine_ls_goodness_of_fit_all   2.53
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_restraints     82
_refine_ls_R_Fsqd_factor         0.06952
_refine_ls_shift/su_max          0.05
_refine_ls_shift/su_mean         0.01
_reflns_d_resolution_high        1.199
_reflns_d_resolution_low         11.240
_reflns_limit_h_max              9
_reflns_limit_h_min              0
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              5
_reflns_limit_l_min              -5
_reflns_number_total             1138
_cod_data_source_file            cg070058q-file004.cif
_cod_data_source_block           1A-120_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 (82
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 (39 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        935.30(5)
_cod_original_sg_symbol_H-M      'p 21/c'
_cod_database_code               4503050
_refine_ls_r_f_factor            0.0485
_gsas_exptl_extinct_corr_t_min   1.00000
_gsas_exptl_extinct_corr_t_max   1.00000