Dissociation of 2,4-Bis(2,4,6-tri-tert-butylphenyl)-cyclo-1,3-dipnicta-2,4-diazanes (pnict = P, As, Sb) Imposed by Substituent Steric Strain: A Cyclobutane/Olefin Analogy
Neil Burford; T. Stanley Cameron; Charles L. B. Macdonald; Katherine N. Robertson; Robert Schurko; Denise Walsh; Robert McDonald; Roderick E. Wasylishen; Inorganic Chemistry 44 (2005) 8058–8064; doi:10.1021/ic050770h

data_4309842
_publ_contact_author_address
;
Department of Chemistry
Dalhousie University
Halifax, Nova Scotia
B3H 4J3
Canada
;
_publ_contact_author_email       ' neil.burford@dal.ca '
_publ_contact_author_fax         ' (902) 494-1310 '
_publ_contact_author_name        ' Neil Burford'
_publ_contact_author_phone       ' (902) 494-3190 '
_publ_section_title
;
Dissociation of
2,4-Bis(2,4,6-tri-tert-butylphenyl)-cyclo-1,3-dipnicta-2,4-diazanes (pnict
= P, As, Sb) Imposed by Substituent Steric Strain: A Cyclobutane/Olefin
Analogy
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8058
_journal_page_last               8064
_journal_paper_doi               10.1021/ic050770h
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C38 H58 F6 N2 O6 P2 S2'
_chemical_formula_sum            'C38 H58 F6 N2 O6 P2 S2'
_chemical_formula_weight         878.92
_chemical_name_systematic
;
 ?
;
_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                 90.59(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.368(2)
_cell_length_b                   16.429(3)
_cell_length_c                   12.013(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      22.2
_cell_volume                     2243.5(7)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction
;
teXsan for Windows version 1.06 (MSC, 1997-1999)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_sigmaI/netI    0.1044
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3857
_diffrn_reflns_theta_full        60.10
_diffrn_reflns_theta_max         60.10
_diffrn_reflns_theta_min         2.69
_diffrn_standards_decay_%        -6.79
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.346
_exptl_absorpt_correction_T_max  0.4964
_exptl_absorpt_correction_T_min  0.3299
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North,Phillips & Matthews, 1968
;
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'pale yellow'
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.448
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3323
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.482
_refine_ls_R_factor_all          0.1389
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                1741
_reflns_number_total             3323
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050770hsi20050513_022640_2.cif
_cod_data_source_block           '[Mes*NPOTf]2'
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4309842