Syntheses and X-ray Structures of Potassium Derivatives and a Paramagnetic Nickel(II) Complex of a Cyclodiphosph(III/V)azane Monoselenide
Tristram Chivers; Mark Krahn; Gabriele Schatte; Inorganic Chemistry 41 (2002) 4348–4354; doi:10.1021/ic020167o

data_4318393
_publ_contact_author_address
; Department of Chemistry
   University of Calgary
   Calgary Alberta T2N 1N4
   Canada
;
_publ_contact_author_email       chivers@ucalgary.ca
_publ_contact_author_fax         '001 403 289 9488'
_publ_contact_author_name        'Dr Tristram Chivers'
_publ_contact_author_phone       '001 403 220 5741'
_publ_section_title
;
 Syntheses and X-ray Structures of Potassium Derivatives and a
 Paramagnetic Nickel(II) Complex of a Cyclodiphosph(III/V)azane
 Monoselenide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4348
_journal_page_last               4354
_journal_paper_doi               10.1021/ic020167o
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C40 H90 K2 N8 O2 P4 Se2'
_chemical_formula_sum            'C40 H90 K2 N8 O2 P4 Se2'
_chemical_formula_weight         1075.20
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 94.4827(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.6393(11)
_cell_length_b                   9.7769(10)
_cell_length_c                   28.036(3)
_cell_measurement_reflns_used    5740
_cell_measurement_temperature    193(2)
_cell_volume                     2907.4(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  WinGX-1.63
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5804
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        'no deacy'
_exptl_absorpt_coefficient_mu    1.561
_exptl_absorpt_correction_T_max  0.5031
_exptl_absorpt_correction_T_min  0.4301
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;SADABS, V 2.01, Software for Area-Detector Absorption
   Corrections; Bruker AXS Inc., Madison, WI, 2000.
;
_exptl_crystal_colour            prism
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       colourless
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.51
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         5804
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+1.3995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0917
_reflns_number_gt                4680
_reflns_number_total             5804
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020167o_4.cif
_cod_data_source_block           8
_cod_original_sg_symbol_Hall     -P2ybc
_cod_database_code               4318393