Melem- and melamine-derived iminophosphoranes
Saplinova, Tatyana; Lehnert, Christian; Böhme, Uwe; Wagler, Jörg; Kroke, Edwin; New Journal of Chemistry 34 (2010) 1893–; doi:10.1039/b9nj00621d

data_7053395
_publ_section_title
;
 Melem- and melamine-derived iminophosphoranes
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1893
_journal_paper_doi               10.1039/b9nj00621d
_journal_volume                  34
_journal_year                    2010
_chemical_formula_moiety         '0.333(C18 H12 Cl6), C6 Cl9 N10 P3'
_chemical_formula_sum            'C12 H4 Cl11 N10 P3'
_chemical_formula_weight         771.11
_chemical_name_systematic
;
?
;
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   18.0719(3)
_cell_length_b                   18.0719(3)
_cell_length_c                   14.7542(6)
_cell_measurement_reflns_used    3369
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      23.53
_cell_measurement_theta_min      3.05
_cell_volume                     4173.1(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep32 (Farugia)'
_computing_publication_material  'Shelx-97/ciftab(Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11614
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    1.298
_exptl_absorpt_correction_T_max  0.8292
_exptl_absorpt_correction_T_min  0.7272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       piece
_exptl_crystal_F_000             2267.6
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.06(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1829
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0372P)^2^+3.6809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0734
_reflns_number_gt                1638
_reflns_number_total             1829
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b9nj00621d.txt
_cod_data_source_block           jw_ts0501
_cod_original_sg_symbol_H-M      R3c
_cod_database_code               7053395