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_4309841
_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         'C18 H29 As Cl N '
_chemical_formula_sum            'C18 H29 As Cl N'
_chemical_formula_weight         369.81
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 107.343(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.088(2)
_cell_length_b                   9.614(1)
_cell_length_c                   16.7819(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      37.2
_cell_measurement_theta_min      32.4
_cell_volume                     1861.6(4)
_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
;
SIR92 (Altomare, et. al. 1994)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.00978
_diffrn_orient_matrix_UB_12      0.09433
_diffrn_orient_matrix_UB_13      -0.02630
_diffrn_orient_matrix_UB_21      -0.02350
_diffrn_orient_matrix_UB_22      -0.04383
_diffrn_orient_matrix_UB_23      -0.05661
_diffrn_orient_matrix_UB_31      -0.08284
_diffrn_orient_matrix_UB_32      0.00129
_diffrn_orient_matrix_UB_33      -0.00030
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0655
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3401
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        63.53
_diffrn_reflns_theta_max         63.53
_diffrn_reflns_theta_min         2.76
_diffrn_standards_decay_%        -0.17
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.727
_exptl_absorpt_correction_T_max  0.6858
_exptl_absorpt_correction_T_min  0.5071
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North,Phillips & Mathews (1968)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             776.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.00164(14)
_refine_ls_extinction_expression
;
Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
;
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3024
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0404P)^2^+2.0803P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.1101
_reflns_number_gt                1803
_reflns_number_total             3024
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            ic050770hsi20050513_022640_1.cif
_cod_data_source_block           '[Mes*NAsCl]2_decomposition_product'
_cod_original_cell_volume        1861.6(3)
_cod_original_sg_symbol_Hall     '-P 2yab '
_cod_original_sg_symbol_H-M      'P 21/a '
_cod_original_formula_sum        'C18 H29 As Cl N '
_cod_database_code               4309841