Zinc, Cadmium, and Mercury Complexes of a Pyridyloxy-Substituted Cyclotriphosphazene: Syntheses, Structures, and Fluxional Behavior
Eric W. Ainscough; Andrew M. Brodie; Patrick J. B. Edwards; Geoffrey B. Jameson; Carl A. Otter; Stephen Kirk; Inorganic Chemistry 51 (2012) 10884–10892; doi:10.1021/ic3013574

data_4330651
_publ_contact_author_address
;
 Chemistry-Institute of Fundamental Sciences, Massey University, 
 Private Bag 11222, Palmerston North, New Zealand
;
_publ_contact_author_email       A.Brodie@massey.ac.nz
_publ_section_title
;
 Zinc, Cadmium, and Mercury Complexes of a Pyridyloxy-Substituted
 Cyclotriphosphazene: Syntheses, Structures, and Fluxional Behavior
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10884
_journal_page_last               10892
_journal_paper_doi               10.1021/ic3013574
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
'3[C36 H32 Cd Cl2 N7 O6 P3] 2.75[C H2 Cl2] 0.25[H2 O] 0.375[C6 H14]'
_chemical_formula_sum            'C113 H107.25 Cd3 Cl11.5 N21 O18.25 P9'
_chemical_formula_weight         3075.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.811(2)
_cell_angle_beta                 94.710(2)
_cell_angle_gamma                101.398(2)
_cell_formula_units_Z            2
_cell_length_a                   13.8423(5)
_cell_length_b                   17.6519(7)
_cell_length_c                   27.6057(11)
_cell_measurement_temperature    93(2)
_cell_volume                     6586.7(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'area detector'
_diffrn_measurement_method       '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  0.0769
_diffrn_reflns_av_sigmaI/netI    0.0852
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            76797
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Acta Cryst, 1995, A51, 33-38'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_description       prism
_exptl_crystal_F_000             3106
_exptl_crystal_size_max          0.77
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.330
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.00064(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1692
_refine_ls_number_reflns         22565
_refine_ls_number_restraints     745
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0217P)^2^+20.6666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1128
_reflns_number_gt                16489
_reflns_number_total             22565
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3013574_si_003_3.cif
_cod_data_source_block           skb
_cod_database_code               4330651