Click Synthesis of Fluorine-Rich Cyclotriphosphazene Hydrazones. Synthesis and Supramolecular Structures of N3P3(N(Me)NCHC6F5)6,spiro-N3P3(C12H8O2)(N(Me)NCHC6F5)4, anddispiro-N3P3(C12H8O2)2(N(Me)NCHC6F5)2
Chandrasekhar, Vadapalli; Thilagar, Pakkirisamy; Krishnan, Venkatasubbaiah; Bickley, James. F.; Steiner, Alexander; Crystal Growth & Design 7 (2007) 668–; doi:10.1021/cg060496h

data_4503939
_publ_section_title
;
 Click Synthesis of Fluorine-Rich Cyclotriphosphazene Hydrazones.
 Synthesis and Supramolecular Structures of
 N3P3(N(Me)NCHC6F5)6,spiro-N3P3(C12H8O2)(N(Me)NCHC6F5)4,
 anddispiro-N3P3(C12H8O2)2(N(Me)NCHC6F5)2
;
_journal_issue                   4
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              668
_journal_paper_doi               10.1021/cg060496h
_journal_volume                  7
_journal_year                    2007
_chemical_formula_sum            'C44 H24 F20 N11 O2 P3'
_chemical_formula_weight         1211.65
_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                 106.583(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5169(14)
_cell_length_b                   12.7823(10)
_cell_length_c                   21.6880(18)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      -28.0
_cell_volume                     4654.1(6)
_computing_cell_refinement       'Bruker SMART V5.628'
_computing_data_collection       'Bruker SMART V5.628'
_computing_data_reduction        'Bruker SAINT+ V6.45'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      546(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0577
_diffrn_reflns_av_sigmaI/netI    0.0813
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            30481
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.263
_exptl_absorpt_correction_T_max  0.9742
_exptl_absorpt_correction_T_min  0.9493
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            'COLOR LESS'
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     853
_refine_ls_number_reflns         11504
_refine_ls_number_restraints     438
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1158
_refine_ls_R_factor_gt           0.0731
_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^)+(0.0453P)^2^+6.2098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1567
_reflns_number_gt                7828
_reflns_number_total             11504
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg060496hsi20070102_062547.cif
_cod_data_source_block           compound5
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4503939