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_7215366
_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            'C54 H30 N3 O6 P3'
_chemical_formula_weight         909.72
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 102.120(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.909(2)
_cell_length_b                   31.013(4)
_cell_length_c                   9.0740(10)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.53
_cell_measurement_theta_min      1.9
_cell_volume                     4102.1(9)
_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 0.864
_diffrn_measured_fraction_theta_max 0.864
_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  0.0587
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            35280
_diffrn_reflns_theta_full        33.53
_diffrn_reflns_theta_max         33.53
_diffrn_reflns_theta_min         1.90
_diffrn_source_type              'ID23-2 gemini-microfocus'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.207
_exptl_crystal_colour            none
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.004
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         7523
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0577P)^2^+2.1495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1081
_reflns_number_gt                6340
_reflns_number_total             7523
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce05529a.txt
_cod_data_source_block           MRM26b
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7215366