Phosphazene vs.diazaphospholene PN-bond cleavage in spirocyclic cyclodiphosphazenes
Burck, Sebastian; Gudat, Dietrich; Nieger, Martin; Schalley, Christoph A.; Weilandt, Torsten; Dalton Transactions  (2008) 3478–3485; doi:10.1039/b717219b

data_7003568
_publ_section_title
;
 Phosphazene vs.diazaphospholene PN-bond cleavage in spirocyclic
 cyclodiphosphazenes
;
_journal_issue                   26
_journal_name_full               'Dalton Transactions'
_journal_page_first              3478
_journal_page_last               3485
_journal_paper_doi               10.1039/b717219b
_journal_year                    2008
_chemical_formula_moiety         'C56 H82 N6 O P2, (C7 H8)2'
_chemical_formula_sum            'C70 H98 N6 O P2'
_chemical_formula_weight         1101.48
_chemical_name_common
;
1,3-Bis-(2,6-diisopropylphenyl)-4,5-dimethyl-2-(1,3-bis-(2,6-
diisopropyl-phenyl)-4,5-dimethyl-2-oxo-2lambda5-1,3,2-
diazaphospholenylimino)-2lambda5-1,3,2-diazaphospholenylamine
;
_chemical_name_systematic
;
1,3-Bis-(2,6-diisopropylphenyl)-4,5-dimethyl-2-[1,3-bis-(2,6-diisopropyl-
phenyl)-4,5-dimethyl-2-oxo-2lambda5-1,3,2-diazaphospholenylimino]-
2lambda5-1,3,2-diazaphospholenylamine
;
_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                102.26(3)
_cell_angle_beta                 103.09(3)
_cell_angle_gamma                99.46(3)
_cell_formula_units_Z            2
_cell_length_a                   13.279(3)
_cell_length_b                   14.542(3)
_cell_length_c                   17.751(4)
_cell_measurement_reflns_used    56
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     3180.3(14)
_computing_cell_refinement       DIRAX
_computing_data_collection       Collect
_computing_data_reduction        EVALCCD
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       'rotation in phi and omega, 1 deg.'
_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  0.1027
_diffrn_reflns_av_sigmaI/netI    0.1504
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37376
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         11069
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1805
_refine_ls_R_factor_gt           0.0794
_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^)+(0.1003P)^2^+1.7006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.2192
_reflns_number_gt                5557
_reflns_number_total             11069
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b717219b.txt
_cod_data_source_block           dg019_hy_compound_5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3180.2(12)
_cod_database_code               7003568