Bis(<i>N</i>,<i>N</i>',<i>N</i>''-triisopropylguanidinium) fumarate–fumaric acid (1/1)
Said, Farouq F.; Ali, Basem F.; Richeson, Darrin; Korobkov, Ilia; Acta Crystallographica Section E 68 (2012) o1906–; doi:10.1107/S1600536812023094

data_2235201
_publ_section_title
;
 Bis(<i>N</i>,<i>N</i>',<i>N</i>''-triisopropylguanidinium)
 fumarate--fumaric acid (1/1)
;
_journal_coeditor_code           PV2540
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1906
_journal_paper_doi               10.1107/S1600536812023094
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '2C10 H24 N3 +, C4 H2 O4 2-, C4 H4 O4'
_chemical_formula_moiety         '2(C10 H24 N3 +), C4 H2 O4 2-, C4 H4 O4'
_chemical_formula_sum            'C28 H54 N6 O8'
_chemical_formula_weight         602.78
_chemical_name_systematic
;
Bis(<i>N</i>,<i>N</i>',<i>N</i>''-triisopropylguanidinium) fumarate--fumaric
acid (1/1)
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.291(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.714(3)
_cell_length_b                   11.633(3)
_cell_length_c                   16.226(4)
_cell_measurement_reflns_used    309
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      23.27
_cell_measurement_theta_min      2.17
_cell_volume                     1791.6(8)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'phi and 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  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11184
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.9641
_exptl_absorpt_correction_T_min  0.9602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.181
_refine_ls_extinction_coef       0.013(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2514
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0727P)^2^+0.7515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1300
_reflns_number_gt                2121
_reflns_number_total             2514
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            pv2540.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

2019-10-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_moiety     'C10 H24 N3 +, 0.5(C4 H2 O4 2-), 0.5(C4 H4 O4)'
_cod_original_formula_iupac      'C10 H24 N3 +, 0.5C4 H2 O4 2-, 0.5C4 H4 O4'
_cod_original_formula_sum        'C14 H27 N3 O4'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     301.39
_cod_database_code               2235201
_cod_database_fobs_code          2235201