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_7031262
_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         'C20 H47 N6 P2 Se2, 0.5(O H2), 2I'
_chemical_formula_sum            'C20 H47 I2 N6 O0.5 P2 Se2'
_chemical_formula_weight         853.29
_chemical_name_systematic
;
4-[1,3-di-<i>tert</i>-butyl-4-(4,4-dimethylpiperazin-4-ium-1-
yl)-2,4-diselanylidene-1,3,2\l^5^,4\l^5^-diazadiphosphedin-2-
yl]-1,1-dimethylpiperazin-1-ium iodide hydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 107.558(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.556(3)
_cell_length_b                   9.5372(10)
_cell_length_c                   21.679(2)
_cell_measurement_reflns_used    9118
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.23
_cell_volume                     6417.6(11)
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0690
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            110101
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        28.300
_diffrn_reflns_theta_max         28.333
_diffrn_reflns_theta_min         2.011
_exptl_absorpt_coefficient_mu    4.350
_exptl_absorpt_correction_T_max  0.5933
_exptl_absorpt_correction_T_min  0.5483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3336
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.134
_exptl_transmission_factor_max   0.727
_exptl_transmission_factor_min   0.551
_refine_diff_density_max         2.042
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         15994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+13.9217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1038
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13166
_reflns_number_total             15994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt00801d2.cif
_cod_data_source_block           msb310_sq_s
_cod_depositor_comments
;

2017-03-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        6417.7(11)
_cod_original_formula_moiety     'C40 H94 N12 P4 Se4, O, 4I'
_cod_original_formula_sum        'C40 H94 I4 N12 O P4 Se4'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1706.59
_cod_database_code               7031262
_shelx_estimated_absorpt_t_min   0.548
_shelx_estimated_absorpt_t_max   0.593
_shelxl_version_number           2013-3
_shelx_res_checksum              38501