Solvent inclusion in the crystal structure of bis[(adamantan-1-yl)methanaminium chloride] 1,4-dioxane hemisolvate monohydrate explained using the computed crystal energy landscape
Mohamed, Sharmarke; Acta Crystallographica Section E 72 (2016) 1348–1352; doi:10.1107/S2056989016013256

data_2241824
_publ_section_title
;
 Solvent inclusion in the crystal structure of
 bis[(adamantan-1-yl)methanaminium chloride] 1,4-dioxane hemisolvate
 monohydrate explained using the computed crystal energy landscape
;
_journal_coeditor_code           HB7608
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1348
_journal_page_last               1352
_journal_paper_doi               10.1107/S2056989016013256
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C11 H20 N + ,Cl - , 0.25C4 H8 O2 , 0.5H2 O'
_chemical_formula_moiety         'Cl, 0.5(H2 O), C11 H20 N, 0.25(C4 H8 O2)'
_chemical_formula_sum            'C12 H23 Cl N O'
_chemical_formula_weight         465.53
_chemical_name_systematic
;
Bis[(adamantan-1-yl)methanaminium chloride]
1,4-dioxane hemisolvate monohydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                102.911(3)
_cell_angle_beta                 91.824(3)
_cell_angle_gamma                101.500(3)
_cell_formula_units_Z            4
_cell_length_a                   6.4941(11)
_cell_length_b                   13.491(2)
_cell_length_c                   15.086(3)
_cell_measurement_reflns_used    4531
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      28.026
_cell_measurement_theta_min      2.340
_cell_volume                     1258.4(4)
_computing_cell_refinement
;
SAINT (Bruker 2015)
;
_computing_data_collection
;
APEX2 (Bruker 2015)
;
_computing_data_reduction
;
SAINT (Bruker 2015)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2008)
;
_computing_structure_solution
;
XT (Sheldrick, 2015)
;
_diffrn_ambient_temperature      100.0(10)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0961
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35014
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.441
_diffrn_reflns_theta_min         1.585
_exptl_absorpt_coefficient_mu    0.280
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2015)
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       needle
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.390
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         6312
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0562
_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^)+(0.0415P)^2^+0.1332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.1047
_reflns_number_gt                4285
_reflns_number_total             6312
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7608sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2019-10-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        1258.5(4)
_cod_original_formula_moiety     '2(Cl), H2 O, 2(C11 H20 N), 0.5(C4 H8 O2)'
_cod_original_formula_iupac      '2C11 H20 N + ,2Cl - , 0.5C4 H8 O2 , H2 O'
_cod_original_formula_sum        'C24 H46 Cl2 N2 O2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     465.53
_cod_database_code               2241824
_cod_database_fobs_code          2241824
_shelx_hkl_checksum              42291
_shelx_res_checksum              59331