Bis(adamantan-1-aminium) hydrogen phosphate fumaric acid sesquisolvate
Mrad, Mohamed Lahbib; Zeller, Matthias; Hernandez, Kristen J.; Rzaigui, Mohamed; Ben Nasr, Cherif; Acta Crystallographica Section E 68 (2012) o2531–o2532; doi:10.1107/S1600536812032734

data_2236013
_publ_section_title
;
 Bis(adamantan-1-aminium) hydrogen phosphate fumaric acid sesquisolvate
;
_journal_coeditor_code           WM2659
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2531
_journal_page_last               o2532
_journal_paper_doi               10.1107/S1600536812032734
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '4C10 H18 N +, 2H O4 P 2-, 3C4 H4 O4'
_chemical_formula_moiety         '4(C10 H18 N +), 2(H O4 P 2-), 3(C4 H4 O4)'
_chemical_formula_sum            'C52 H86 N4 O20 P2'
_chemical_formula_weight         1149.18
_chemical_name_systematic
;
Bis(adamantan-1-aminium) hydrogen phosphate fumaric acid sesquisolvate
;
_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                 105.795(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.7555(16)
_cell_length_b                   11.1850(14)
_cell_length_c                   20.251(2)
_cell_measurement_reflns_used    6149
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.50
_cell_measurement_theta_min      2.46
_cell_volume                     2780.1(6)
_computing_cell_refinement       'SAINT (Bruker, 2011)'
_computing_data_collection       'APEX2 (Bruker, 2011)'
_computing_data_reduction        'SAINT (Bruker, 2011)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXLE (H\"ubschle <i>et al.</i>, 2011)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\w 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  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24141
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         32.20
_diffrn_reflns_theta_min         1.70
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2011)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.392
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         9001
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0581P)^2^+0.6840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1133
_reflns_number_gt                7424
_reflns_number_total             9001
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm2659.cif
_cod_data_source_block           I
_cod_depositor_comments
;

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     '2(C10 H18 N +), H O4 P 2-, 1.5(C4 H4 O4)'
_cod_original_formula_iupac      '2C10 H18 N +, H O4 P 2-, 1.5C4 H4 O4'
_cod_original_formula_sum        'C26 H43 N2 O10 P'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     574.59
_cod_database_code               2236013
_cod_database_fobs_code          2236013