A combined crystallographic and theoretical study of weak intermolecular interactions in crystalline squaric acid esters and amides
Prohens, Rafel; Frontera, Antonio; Portell, Anna; Font-Bardia, Merce; Bauza, Antonio; CrystEngComm  (2017) –; doi:10.1039/C7CE00556C

data_7228238
_publ_section_title
;
 A combined crystallographic and theoretical study of weak intermolecular
 interactions in crystalline squaric acid esters and amides
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00556C
_journal_year                    2017
_chemical_formula_moiety         'C20 H20 N2 O4, 4/5(C2 H6 O S), 2/5(H2 O)'
_chemical_formula_sum            'C21.6 H25.6 N2 O5.2 S0.8'
_chemical_formula_weight         422.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/cc13597t
_audit_creation_method           SHELXL-2012
_audit_update_record
;
2014-08-05 deposited with the CCDC.
2017-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.764(10)
_cell_angle_gamma                90
_cell_formula_units_Z            20
_cell_length_a                   23.485(10)
_cell_length_b                   9.632(4)
_cell_length_c                   47.030(19)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    303(2)
_cell_measurement_theta_max      21.83
_cell_measurement_theta_min      2.32
_cell_volume                     10564(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      303(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            173437
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.115
_diffrn_reflns_theta_min         2.159
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       prism
_exptl_crystal_F_000             4472
_exptl_crystal_size_max          0.576
_exptl_crystal_size_mid          0.308
_exptl_crystal_size_min          0.189
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.166
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.703
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1353
_refine_ls_number_reflns         27354
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.704
_refine_ls_R_factor_all          0.3231
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0520
_refine_ls_wR_factor_ref         0.0856
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6230
_reflns_number_total             27354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00556c2.cif
_cod_data_source_block           mo_023SB127B_0ma_aa
_cod_depositor_comments
;

2017-11-21
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '5(C20 H20 N2 O4), 4(C2 H6 O S), 2(H2 O)'
_cod_original_formula_sum        'C108 H128 N10 O26 S4'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     2110.44
_cod_database_code               7228238
_shelxl_version_number           2012-9
_shelx_res_checksum              41636