2,8,9-Tris(2-methylpropyl)-2,5,8,9-tetraaza-1λ^5^-phosphatricyclo[3.3.3.0^1,5^]undecan-5-ium chloride dihydrate
Lee, Junseong; Kim, Youngjo; Acta Crystallographica Section E 68 (2012) o3317–; doi:10.1107/S1600536812045618

data_2236854
_publ_section_title
;
 2,8,9-Tris(2-methylpropyl)-2,5,8,9-tetraaza-1\l^5^-phosphatricyclo[3.3.3.0^1,5^]undecan-5-ium
 chloride dihydrate
;
_journal_coeditor_code           FF2086
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3317
_journal_paper_doi               10.1107/S1600536812045618
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C18 H40 N4 P +, Cl -, 2H2 O'
_chemical_formula_moiety         'C18 H40 N4 P +, Cl -, 2(H2 O)'
_chemical_formula_sum            'C18 H44 Cl N4 O2 P'
_chemical_formula_weight         414.99
_chemical_name_systematic
;
2,8,9-Tris(2-methylpropyl)-2,5,8,9-tetraaza-1\l^5^-
phosphatricyclo[3.3.3.0^1,5^]undecan-5-ium chloride dihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.720(8)
_cell_angle_beta                 92.259(8)
_cell_angle_gamma                90.616(8)
_cell_formula_units_Z            4
_cell_length_a                   10.0945(19)
_cell_length_b                   15.759(3)
_cell_length_c                   16.122(3)
_cell_measurement_reflns_used    4603
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.85
_cell_measurement_theta_min      2.14
_cell_volume                     2453.7(8)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \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  0.0628
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35181
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.64
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_T_max  0.9673
_exptl_absorpt_correction_T_min  0.9538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.307
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         9856
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1299
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1089P)^2^+0.2470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1745
_refine_ls_wR_factor_ref         0.2124
_reflns_number_gt                5364
_reflns_number_total             9856
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ff2086.cif
_cod_data_source_block           I
_cod_original_cell_volume        2453.6(8)
_cod_original_formula_sum        'C18 H44 Cl1 N4 O2 P1'
_cod_database_code               2236854
_cod_database_fobs_code          2236854