A new class of azadipnictiridines generated by an unusual rearrangement reaction.
Hinz, Alexander; Schulz, Axel; Seidel, Wolfram W.; Villinger, Alexander; Inorganic chemistry 53 (2014) 11682–11690; doi:10.1021/ic501905v

data_4341335
_publ_section_title
;
 A new class of azadipnictiridines generated by an unusual rearrangement
 reaction.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11682
_journal_page_last               11690
_journal_paper_doi               10.1021/ic501905v
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C64 H64 N2 P2 S2, 2(C6 H14)'
_chemical_formula_sum            'C76 H92 N2 P2 S2'
_chemical_formula_weight         1159.58
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/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                 107.923(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.8066(9)
_cell_length_b                   17.9402(15)
_cell_length_c                   17.4153(14)
_cell_measurement_reflns_used    3000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      44.276
_cell_measurement_theta_min      4.343
_cell_volume                     3509.8(5)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_av_sigmaI/netI    0.1562
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24603
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_T_max  0.9839
_exptl_absorpt_correction_T_min  0.9513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
The unit cell contains four n-hexane molecules which have been treated 
as a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.104
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         7880
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.1500
_refine_ls_R_factor_gt           0.0768
_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^)+(0.0968P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1870
_refine_ls_wR_factor_ref         0.2082
_reflns_number_gt                3672
_reflns_number_total             7880
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic501905v_si_002.cif
_cod_data_source_block           ah021d_2
_cod_depositor_comments
'Adding full bibliography for 4341335--4341344.cif.'
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               4341335