({-})-Sparteinium tetrachloridozincate monohydrate
Bernès, Sylvain; Gutiérrez, René; Hernández-Téllez, Guadalupe; Moreno, Gloria E.; IUCrData 1 (2016) x161237–; doi:10.1107/S2414314616012372

data_1543877
_publ_section_title
;
 ({-})-Sparteinium tetrachloridozincate monohydrate
;
_journal_coeditor_code           WM4021
_journal_issue                   8
_journal_name_full               IUCrData
_journal_page_first              x161237
_journal_paper_doi               10.1107/S2414314616012372
_journal_volume                  1
_journal_year                    2016
_chemical_formula_iupac          '(C15 H28 N2) [Zn Cl4], H2 O'
_chemical_formula_moiety         'C15 H28 N2 2+, Cl4 Zn 2-, H2 O'
_chemical_formula_sum            'C15 H30 Cl4 N2 O Zn'
_chemical_formula_weight         461.58
_chemical_name_common
;
(-)-Sparteinium tetrachloridozincate monohydrate
;
_chemical_name_systematic
;
(-)-7,15-Diazatetracyclo[7.7.1.0^2,7^.0^10,15^]heptadecane-7,15-diium
tetrachloridozincate monohydrate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     isomor
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4549(6)
_cell_length_b                   14.7691(10)
_cell_length_c                   16.3607(9)
_cell_measurement_reflns_used    65
_cell_measurement_temperature    297.0(10)
_cell_measurement_theta_max      14.02
_cell_measurement_theta_min      4.64
_cell_volume                     2043.0(2)
_computing_cell_refinement
;
XSCANS (Bruker, 1997)
;
_computing_data_collection
;
XSCANS (Bruker, 1997)
;
_computing_data_reduction
;
XSCANS (Bruker, 1997)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
'coordinates taken from an isostructural compound'
_diffrn_ambient_temperature      297.0(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            4207
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         1.858
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.730
_exptl_absorpt_correction_T_max  0.277
_exptl_absorpt_correction_T_min  0.210
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
(XSCANS; Bruker, 1997)
;
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.267
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 593 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.004(11)
_refine_ls_extinction_coef       0.0095(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3989
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0265
_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^)+(0.0309P)^2^+0.3509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0679
_reflns_number_gt                3673
_reflns_number_total             3989
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm4021sup1.cif
_cod_data_source_block           I
_cod_database_code               1543877
_shelx_hkl_checksum              89669
_shelx_res_checksum              88087
_cod_database_fobs_code 1543877