Hydrogen-bonding adducts of benzenepolycarboxylic acids with <i>N</i>,<i>N</i>-dimethylformamide: benzene-1,4-dicarboxylic acid <i>N</i>,<i>N</i>-dimethylformamide disolvate, benzene-1,2,4,5-tetracarboxylic acid <i>N</i>,<i>N</i>-dimethylformamide tetrasolvate and benzene-1,2,3-tricarboxylic acid <i>N</i>,<i>N</i>-dimethylformamide disolvate monohydrate
Dale, Sophie H.; Elsegood, Mark R.J.; Acta Crystallographica Section C 60 (2004) o444–o448; doi:10.1107/S010827010400976X

data_2013968
_publ_section_title
;
 Hydrogen-bonding adducts of benzenepolycarboxylic acids with
 <i>N</i>,<i>N</i>-dimethylformamide: benzene-1,4-dicarboxylic acid
 <i>N</i>,<i>N</i>-dimethylformamide disolvate,
 benzene-1,2,4,5-tetracarboxylic acid
 <i>N</i>,<i>N</i>-dimethylformamide tetrasolvate and
 benzene-1,2,3-tricarboxylic acid <i>N</i>,<i>N</i>-dimethylformamide
 disolvate monohydrate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o444
_journal_page_last               o448
_journal_paper_doi               10.1107/S010827010400976X
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C10 H6 O8, 4C3 H7 N O'
_chemical_formula_moiety         'C10 H6 O8, 4C3 H7 N O'
_chemical_formula_sum            'C22 H34 N4 O12'
_chemical_formula_weight         546.53
_chemical_name_systematic
;
benzene-1,2,4,5-tetracarboxylic acid N,N-dimethylformamide tetrasolvate
;
_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 except OH coords freely refined'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.162(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.8905(10)
_cell_length_b                   7.9398(6)
_cell_length_c                   13.8078(10)
_cell_measurement_reflns_used    5456
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.56
_cell_measurement_theta_min      2.61
_cell_volume                     1342.79(18)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2000)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_sigmaI/netI    0.0176
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11290
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.88
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2001)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+0.3704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.1000
_reflns_number_gt                2522
_reflns_number_total             3213
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg1747.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (9 times).

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

The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (9 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1342.79(17)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2013968
_cod_database_fobs_code          2013968