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_4307657
_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            'C74 H50 Cl8 N8 O12 P8'
_chemical_formula_weight         1774.58
_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                105.0690(10)
_cell_angle_beta                 97.0330(10)
_cell_angle_gamma                93.2880(10)
_cell_formula_units_Z            2
_cell_length_a                   12.34300(10)
_cell_length_b                   15.49710(10)
_cell_length_c                   20.7351(3)
_cell_measurement_temperature    293(2)
_cell_volume                     3784.53(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33237
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  0.8733
_exptl_absorpt_correction_T_min  0.8389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Acta Cryst., 1995, A51, 33'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.224
_refine_diff_density_min         -1.261
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1001
_refine_ls_number_reflns         13739
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.209
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+10.1371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1328
_reflns_number_gt                10341
_reflns_number_total             13739
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062141tsi20061113_035514_4.cif
_cod_data_source_block           3BC
_cod_database_code               4307657