Bis(oxotremorine) fumarate bis(fumaric acid)
Naeem, Marilyn; Chadeayne, Andrew R.; Golen, James A.; Manke, David R.; IUCrData 7 (2022) x220364–; doi:10.1107/S2414314622003649

data_1566768
_publ_section_title
;
 Bis(oxotremorine) fumarate bis(fumaric acid)
;
_journal_coeditor_code           ZL4049
_journal_issue                   4
_journal_name_full               IUCrData
_journal_page_first              x220364
_journal_paper_doi               10.1107/S2414314622003649
_journal_volume                  7
_journal_year                    2022
_chemical_formula_iupac          '2C12 H19 N2 O +, C4 H2 O4 2-, 2C4 H4 O4'
_chemical_formula_moiety         '2(C12 H19 N2 O +), C4 H2 O4 2-, 2(C4 H4 O4)'
_chemical_formula_sum            'C36 H48 N4 O14'
_chemical_formula_weight         760.78
_chemical_name_common
;
Bis(oxotremorine) fumarate bis(fumaric acid)
;
_chemical_name_systematic
;
1-[4-(2-Oxopyrrolidin-1-yl)but-2-ynyl]pyrrolidinium
(2<i>E</i>)-but-2-enedioate bis[(2<i>E</i>)-but-2-enedioic acid]
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_cell_angle_alpha                94.922(2)
_cell_angle_beta                 90.428(2)
_cell_angle_gamma                98.945(2)
_cell_formula_units_Z            1
_cell_length_a                   6.0921(3)
_cell_length_b                   8.5778(5)
_cell_length_c                   18.7260(11)
_cell_measurement_reflns_used    9070
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      25.74
_cell_measurement_theta_min      2.56
_cell_volume                     962.88(9)
_computing_cell_refinement
;
SAINT (Bruker, 2018)
;
_computing_data_collection
;
APEX3 (Bruker, 2018)
;
_computing_data_reduction
;
SAINT (Bruker, 2018)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      297.15
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker D8 Venture CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27417
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.765
_diffrn_reflns_theta_min         2.560
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.7167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2018)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       block
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.182
_refine_diff_density_min         -0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3651
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+0.2757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1089
_reflns_number_gt                2975
_reflns_number_total             3651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl4049sup1.cif
_cod_data_source_block           I
_cod_database_code               1566768
_cod_database_fobs_code          1566768
_shelx_estimated_absorpt_t_min   0.970
_shelx_estimated_absorpt_t_max   0.996
_shelx_hkl_checksum              78103
_shelx_res_checksum              58770