Quaternization and oxidation reactions of cyclodiphosphazane derivatives and their copper(i) and gold(i) complexes.
Balakrishna, Maravanji S.; Suresh, Devarajan; Ananthnag, Guddekoppa S.; Mague, Joel T.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 8835–8848; doi:10.1039/c4dt00801d

data_7031261
_publ_section_title
;
 Quaternization and oxidation reactions of cyclodiphosphazane derivatives
 and their copper(i) and gold(i) complexes.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8835
_journal_page_last               8848
_journal_paper_doi               10.1039/c4dt00801d
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C24 H49 N4 P2 Se, I'
_chemical_formula_sum            'C24 H49 I N4 P2 Se'
_chemical_formula_weight         661.47
_chemical_name_systematic
;
1,3-Di-<i>tert</i>-butyl-2,4-bis-<i>tert</i>-butylamino-
2-methyl-4-selenoxo-4\l^5^-[1,3,2,4]diazadiphosphetidin-
2-ium iodide toluene solvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                93.176(1)
_cell_angle_beta                 104.556(1)
_cell_angle_gamma                91.995(1)
_cell_formula_units_Z            2
_cell_length_a                   9.3436(6)
_cell_length_b                   10.3905(7)
_cell_length_c                   16.7060(13)
_cell_measurement_reflns_used    6895
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.29
_cell_volume                     1565.43(19)
_computing_cell_refinement       'Bruker <i>SMART</i> (Bruker, 2000)'
_computing_data_collection       'Bruker <i>SMART</i> (Bruker, 2000)'
_computing_data_reduction        'Bruker </i>SAINT</i> (Bruker, 2004)'
_computing_molecular_graphics    '<i>DIAMOND</i> (Brandenburg & Putz, 2012)'
_computing_publication_material  'Bruker <i>SHELXTL</i> (Bruker, 2000a)'
_computing_structure_refinement  '<i>SHELXL-2013</i> (Sheldrick, 2013)'
_computing_structure_solution    '<i>SHELXS-97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker-AXS Smart APEX CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0248
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27720
_diffrn_reflns_point_group_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         28.315
_diffrn_reflns_theta_min         2.255
_exptl_absorpt_coefficient_mu    2.305
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '<i>SADABS</i> (Sheldrick, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.142
_exptl_transmission_factor_max   0.750
_exptl_transmission_factor_min   0.649
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Flack x determined using 5960 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.019(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         14366
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0272
_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^)+(0.0124P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0560
_reflns_Friedel_coverage         0.870
_reflns_Friedel_fraction_full    0.889
_reflns_Friedel_fraction_max     0.858
_reflns_number_gt                13574
_reflns_number_total             14366
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt00801d2.cif
_cod_data_source_block           msb304
_cod_database_code               7031261
_shelx_estimated_absorpt_t_min   0.658
_shelx_estimated_absorpt_t_max   0.735
_shelxl_version_number           2013-3
_shelx_res_checksum              58395