1,1',4,5-Tetrahydrotrispiro[1,3,2-diazaphosphole-2,2'-[1,3,5,2,4,6]triazatriphosphinine-4',6''-dibenzo[<i>d</i>,<i>f</i>][1,3,2]dioxaphosphepine-6',6'''-dibenzo[<i>d</i>,<i>f</i>][1,3,2]dioxaphosphepine] acetone monosolvate
Fontenot, Krystal R.; Easson, Michael W.; Fronczek, Frank R.; Condon, Brian D.; Acta Crystallographica Section E 69 (2013) o1491–o1492; doi:10.1107/S1600536813023830

data_2238515
_publ_section_title
;
 1,1',4,5-Tetrahydrotrispiro[1,3,2-diazaphosphole-2,2'-[1,3,5,2,4,6]triazatriphosphinine-4',6''-dibenzo[<i>d</i>,<i>f</i>][1,3,2]dioxaphosphepine-6',6'''-dibenzo[<i>d</i>,<i>f</i>][1,3,2]dioxaphosphepine]
 acetone monosolvate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1491
_journal_page_last               o1492
_journal_paper_doi               10.1107/S1600536813023830
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C26 H22 N5 O4 P3, C3 H6 O'
_chemical_formula_moiety         'C26 H22 N5 O4 P3, C3 H6 O'
_chemical_formula_sum            'C29 H28 N5 O5 P3'
_chemical_formula_weight         619.47
_chemical_name_systematic
'1,1',4,5-Tetrahydrotrispiro[1,3,2-diazaphosphole-2,2'-[1,3,5,2,4,6]triazatriphosphinine-4',6''-dibenzo[<i>d</i>,<i>f</i>][1,3,2]dioxaphosphepine-6',6'''-dibenzo[<i>d</i>,<i>f</i>][1,3,2]dioxaphosphepine] acetone monosolvate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_cell_angle_beta                 97.978(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4901(9)
_cell_length_b                   22.9466(19)
_cell_length_c                   13.1776(13)
_cell_measurement_reflns_used    3314
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      67.78
_cell_measurement_theta_min      3.85
_cell_volume                     2841.9(5)
_computing_cell_refinement       'SAINT (Bruker, 2011)'
_computing_data_collection       'APEX2 (Bruker, 2011)'
_computing_data_reduction        'SAINT (Bruker, 2011)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker Kappa APEXII DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'QUAZAR multilayer optics'
_diffrn_radiation_source         'I\mS microfocus'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            33208
_diffrn_reflns_theta_full        66.60
_diffrn_reflns_theta_max         68.70
_diffrn_reflns_theta_min         3.85
_exptl_absorpt_coefficient_mu    2.344
_exptl_absorpt_correction_T_max  0.9330
_exptl_absorpt_correction_T_min  0.6644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(TWINABS; Sheldrick, 2004)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.386
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         5065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0595P)^2^+0.7869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1022
_reflns_number_gt                4276
_reflns_number_total             5065
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jj2173.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2238515
_cod_database_fobs_code          2238515