Synthesis and crystal structure of tris(2,3-triphenylenedioxy)cyclotriphosphazene: a new clathration system
Reynes, Mathias; Dautel, Olivier J.; Virieux, David; Flot, David; Moreau, Joël J. E.; CrystEngComm 13 (2011) 6050–; doi:10.1039/c1ce05529a

data_7215365
_publ_section_title
;
 Synthesis and crystal structure of
 tris(2,3-triphenylenedioxy)cyclotriphosphazene: a new clathration system
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              6050
_journal_paper_doi               10.1039/c1ce05529a
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C66 H35 Cl6 N3 O6 P3'
_chemical_formula_weight         1271.58
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                94.818(3)
_cell_angle_beta                 99.983(5)
_cell_angle_gamma                98.226(6)
_cell_formula_units_Z            2
_cell_length_a                   8.769(2)
_cell_length_b                   15.024(2)
_cell_length_c                   21.216(2)
_cell_measurement_reflns_used    21428
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.77
_cell_measurement_theta_min      1.2
_cell_volume                     2707.4(8)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       mxCuBE
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_publication_material  'enCIFer, WinGX'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_type            'marMOSAIC 225'
_diffrn_measured_fraction_theta_full 0.869
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_device_type  'ESRF-EMBL MD2M diffractometer'
_diffrn_measurement_method       oscillation
_diffrn_radiation_monochromator  Si111
_diffrn_radiation_source         'ESRF synchrotron'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.87260
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30257
_diffrn_reflns_theta_full        30.77
_diffrn_reflns_theta_max         30.77
_diffrn_reflns_theta_min         1.20
_diffrn_source_type              'ID23-2 gemini-microfocus'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.468
_exptl_crystal_colour            none
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1294
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.086
_refine_diff_density_min         -1.303
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         7949
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0669
_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^)+(0.1163P)^2^+5.3925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1895
_refine_ls_wR_factor_ref         0.1965
_reflns_number_gt                6770
_reflns_number_total             7949
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce05529a.txt
_cod_data_source_block           mrm26a
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7215365