1-Methyl-1-azonia-3,5-diaza-7-phosphatricyclo[3.3.1.1]decane 7-oxide triiodide
Kirillov, Alexander M.; Smoleński, Piotr; Guedes da Silva, M. Fátima C.; Pombeiro, Armando J. L.; Acta Crystallographica Section E 64 (2008) o496–o497; doi:10.1107/S1600536808001426

data_2217576
_publ_section_title
;
 1-Methyl-1-azonia-3,5-diaza-7-phosphatricyclo[3.3.1.1]decane 7-oxide
 triiodide
;
_journal_coeditor_code           KP2159
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o496
_journal_page_last               o497
_journal_paper_doi               10.1107/S1600536808001426
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C7 H15 N3 O P + , I3 -'
_chemical_formula_moiety         'C7 H15 N3 O P + , I3 -'
_chemical_formula_sum            'C7 H15 Cu0 I3 N3 O P'
_chemical_formula_weight         568.89
_chemical_name_systematic
;
1-Methyl-1-azonia-3,5-diaza-7-phosphatricyclo[3.3.1.1]decane 7-oxide
triiodide
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.472(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.1570(8)
_cell_length_b                   8.2257(8)
_cell_length_c                   25.903(3)
_cell_measurement_reflns_used    2835
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      2.6
_cell_volume                     1523.5(3)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>,  2006)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'WinGX (Version 1.70.01; Farrugia, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            11526
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    6.244
_exptl_absorpt_correction_T_max  0.5740
_exptl_absorpt_correction_T_min  0.4974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.441
_refine_diff_density_min         -1.033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0450P)^2^+6.2243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1023
_reflns_number_gt                2214
_reflns_number_total             2789
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            kp2159.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               2217576
_cod_database_fobs_code          2217576