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_4330649
_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_sum            'C38.5 H37 Cl7 N7 O6 P3 Zn'
_chemical_formula_weight         1100.18
_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                97.417(4)
_cell_angle_beta                 104.210(4)
_cell_angle_gamma                111.410(4)
_cell_formula_units_Z            4
_cell_length_a                   14.6984(10)
_cell_length_b                   16.7607(11)
_cell_length_c                   21.9219(15)
_cell_measurement_temperature    97(2)
_cell_volume                     4728.8(6)
_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      97(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  '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  0.0860
_diffrn_reflns_av_sigmaI/netI    0.1000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            53714
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    1.069
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_description       block
_exptl_crystal_F_000             2236
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.492
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1152
_refine_ls_number_reflns         17242
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1366
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0985P)^2^+16.4948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1716
_refine_ls_wR_factor_ref         0.2243
_reflns_number_gt                9937
_reflns_number_total             17242
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3013574_si_003_1.cif
_cod_data_source_block           sk60a
_cod_original_formula_sum        'C38.50 H37 Cl7 N7 O6 P3 Zn'
_cod_database_code               4330649