Conformational Flexibility in 2,2'-Dioxybiphenyl-chloro-cyclotetraphosphazenes and its Relevance to Polyphosphazene Analogues
Eric W. Ainscough; Andrew M. Brodie; Adrian B. Chaplin; Andreas Derwahl; John A. Harrison; Carl A. Otter; Inorganic Chemistry 46 (2007) 2575–2583; doi:10.1021/ic062141t

data_4307658
_publ_contact_author_address
;
 Chemistry-Institute of Fundamental Sciences, Massey University, Private Bag 11222, Palmerston North, New Zealand
;
_publ_contact_author_email       A.M.Brodie@massey.ac.nz
_publ_contact_author_name
;
 Eric w. Ainscough, Andrew M. Brodie, Adrian B. Chaplin,
 Andeas Derwhal, John A. Harrison and Carl A. Otter
;
_publ_section_title
;
Conformational Flexibility in
2,2'-Dioxybiphenyl-chloro-cyclotetraphosphazenes and its Relevance to
Polyphosphazene Analogues
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2575
_journal_page_last               2583
_journal_paper_doi               10.1021/ic062141t
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C36 H24 Cl2 N4 O6 P4'
_chemical_formula_weight         803.37
_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                 95.8800(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.2015(2)
_cell_length_b                   12.05820(10)
_cell_length_c                   20.7909(3)
_cell_measurement_temperature    186(2)
_cell_volume                     3541.60(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  '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  0.1006
_diffrn_reflns_av_sigmaI/netI    0.0791
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30827
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    0.418
_exptl_absorpt_correction_T_max  0.894366
_exptl_absorpt_correction_T_min  0.718637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Acta Cryst., 1995, A51, 33-38'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0581
_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^)+(0.0418P)^2^+5.0201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1268
_reflns_number_gt                4680
_reflns_number_total             6717
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062141tsi20061113_035514_5.cif
_cod_data_source_block           3D
_cod_database_code               4307658