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_4341337
_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         'C60 H76 N2 P2 S2 Si2'
_chemical_formula_sum            'C60 H76 N2 P2 S2 Si2'
_chemical_formula_weight         1007.47
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.284(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.8745(16)
_cell_length_b                   43.059(5)
_cell_length_c                   21.537(3)
_cell_measurement_reflns_used    9774
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      55.590
_cell_measurement_theta_min      4.417
_cell_volume                     11783(3)
_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
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_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0778
_diffrn_reflns_av_sigmaI/netI    0.0786
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       58
_diffrn_reflns_limit_k_min       -57
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            157419
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         0.95
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_T_max  0.9610
_exptl_absorpt_correction_T_min  0.8472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4320
_exptl_crystal_size_max          0.77
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.907
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1283
_refine_ls_number_reflns         30729
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1177
_refine_ls_R_factor_gt           0.0647
_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^)+(0.0613P)^2^+9.2624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1422
_refine_ls_wR_factor_ref         0.1665
_reflns_number_gt                19148
_reflns_number_total             30729
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic501905v_si_002.cif
_cod_data_source_block           ah054a
_cod_depositor_comments
'Adding full bibliography for 4341335--4341344.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4341337