A planar dianionic ditelluride and a cyclic tritelluride supported by P2N2 rings
Nordheider, Andreas; Chivers, Tristram; Thirumoorthi, Ramalingam; Athukorala Arachchige, Kasun S.; Slawin, Alexandra M. Z.; Woollins, J. Derek; Vargas-Baca, Ignacio; Dalton Transactions 42 (2013) 3291–; doi:10.1039/c2dt32716c

data_7020975
_publ_section_title
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 A planar dianionic ditelluride and a cyclic tritelluride supported by
 P2N2 rings
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_journal_issue                   10
_journal_name_full               'Dalton Transactions'
_journal_page_first              3291
_journal_paper_doi               10.1039/c2dt32716c
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C32 H72 N8 Na4 P4, C6 H14'
_chemical_formula_sum            'C38 H86 N8 Na4 P4'
_chemical_formula_weight         870.99
_chemical_name_systematic
;
?
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.51(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.710(4)
_cell_length_b                   21.271(4)
_cell_length_c                   22.414(5)
_cell_measurement_reflns_used    37288
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     9924(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1996)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'KappaCCD (Nonius, FR540C)'
_diffrn_measurement_method       'phi\omega scans'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'Enraf Nonius FR590D, fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0771
_diffrn_reflns_av_sigmaI/netI    0.0870
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19356
_diffrn_reflns_theta_full        21.00
_diffrn_reflns_theta_max         21.00
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.222
_exptl_absorpt_correction_T_max  0.9825
_exptl_absorpt_correction_T_min  0.9425
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (SHELXTL-NT v5.1, Bruker)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3792
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
The Platon SQUEEZE procedure was applied to recover 445 electrons per
unit cell in one void (total volume 1541.3 ^A^3); that is 111 electrons
per formula unit. Lattice solvent hexane molecules (50 electrons/hexane)
were present, and the electrons recovered by SQUEEZE have been assigned
as 2 hexane molecules per formula unit. These hexane molecules have
been included in the formula for the calculation of intensive
properties.
PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13.
;
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     895
_refine_ls_number_reflns         10561
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1330
_refine_ls_R_factor_gt           0.0991
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1613P)^2^+39.7212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2652
_refine_ls_wR_factor_ref         0.2919
_reflns_number_gt                7230
_reflns_number_total             10561
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32716c.txt
_cod_data_source_block           Na4
_cod_depositor_comments
;

2023-11-21
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
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_cod_original_formula_sum            'C76 H172 N16 Na8 P8'
_cod_original_formula_weight         1741.98
_cod_original_formula_moiety         '2(C32 H72 N8 Na4 P4), 2(C6 H14) '
_cod_original_formula_units_Z            4
_cod_original_cell_volume        9924(3)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               7020975