The whole range of hydrogen bonds in one crystal structure: neutron diffraction and charge-density studies of <i>N</i>,<i>N</i>-dimethylbiguanidinium bis(hydrogensquarate)
Şerb, Mihaela-Diana; Wang, Ruimin; Meven, Martin; Englert, Ulli; Acta Crystallographica Section B 67 (2011) 552–559; doi:10.1107/S0108768111043138

data_2105047
_publ_section_title
;
 The whole range of hydrogen bonds in one crystal structure: neutron
 diffraction and charge-density studies of
 <i>N</i>,<i>N</i>-dimethylbiguanidinium bis(hydrogensquarate)
;
_journal_coeditor_code           SO5054
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              552
_journal_page_last               559
_journal_paper_doi               10.1107/S0108768111043138
_journal_volume                  67
_journal_year                    2011
_chemical_formula_moiety         'C4 H13 N5, 2(C4 H O4)'
_chemical_formula_sum            'C12 H15 N5 O8'
_chemical_formula_weight         357.29
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.4259(9)
_cell_angle_beta                 105.1185(9)
_cell_angle_gamma                102.4251(10)
_cell_formula_units_Z            2
_cell_length_a                   7.0689(2)
_cell_length_b                   8.5538(2)
_cell_length_c                   13.0736(3)
_cell_measurement_reflns_used    8412
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.74
_cell_measurement_theta_min      2.44
_cell_volume                     743.58(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0813
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            38327
_diffrn_reflns_theta_full        35.00
_diffrn_reflns_theta_max         52.20
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.436
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         15808
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1055
_reflns_number_gt                9502
_reflns_number_total             15808
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            so5054.cif
_cod_data_source_block           iam
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_database_code               2105047
_cod_database_fobs_code          2105047