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_7053397
_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
'C39 H33 N6 P2, C6 H16 N, 1.5(C6 H4 Cl2), 2(Br)'
_chemical_formula_sum            'C54 H55 Br2 Cl3 N7 P2'
_chemical_formula_weight         1130.16
_chemical_name_systematic
;
?
;
_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                103.179(2)
_cell_angle_beta                 96.281(2)
_cell_angle_gamma                112.2370(10)
_cell_formula_units_Z            2
_cell_length_a                   14.0193(5)
_cell_length_b                   14.1055(6)
_cell_length_c                   15.1516(6)
_cell_measurement_reflns_used    7252
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.72
_cell_measurement_theta_min      2.73
_cell_volume                     2635.91(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP32 (Farugia)'
_computing_publication_material  'Ciftab (Sheldrick)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_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  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29620
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    1.794
_exptl_absorpt_correction_T_max  0.8410
_exptl_absorpt_correction_T_min  0.6886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1158
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         9842
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+0.4182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0825
_reflns_number_gt                7282
_reflns_number_total             9842
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b9nj00621d.txt
_cod_data_source_block           jw_ts01101
_cod_original_cell_volume        2635.91(18)
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7053397