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_4330650
_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            'C37 H34 Cl4 N7 O6 P3 Zn'
_chemical_formula_weight         972.79
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.93(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.512(4)
_cell_length_b                   15.990(3)
_cell_length_c                   14.686(3)
_cell_measurement_temperature    98(2)
_cell_volume                     4107.0(15)
_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      98(2)
_diffrn_measured_fraction_theta_full 0.525
_diffrn_measured_fraction_theta_max 0.525
_diffrn_measurement_device_type  'CCD 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  0.0902
_diffrn_reflns_av_sigmaI/netI    0.0634
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9603
_diffrn_reflns_theta_full        31.23
_diffrn_reflns_theta_max         31.23
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    1.031
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Acta Cryst, 1995, A51, 33-38'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       thin_plate
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         7017
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0572
_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^)+(0.1119P)^2^+0.2030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1506
_refine_ls_wR_factor_ref         0.1642
_reflns_number_gt                5537
_reflns_number_total             7017
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3013574_si_003_2.cif
_cod_data_source_block           sk60
_cod_original_cell_volume        4106.7(14)
_cod_database_code               4330650