Zirconium-Mediated Synthesis of Arsaalkene Compounds from Arsines and Isocyanides
Annalese F. Maddox; Jillian J. Davidson; Tamila Shalumova; Joseph M. Tanski; Rory Waterman; Inorganic Chemistry 52 (2013) 7811–7816; doi:10.1021/ic4012058

data_4335421
_publ_section_title
;
 Zirconium-Mediated Synthesis of Arsaalkene Compounds from Arsines and
 Isocyanides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7811
_journal_page_last               7816
_journal_paper_doi               10.1021/ic4012058
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C31 H56 As N5 Si3 Zr'
_chemical_formula_weight         749.22
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 90.998(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2583(14)
_cell_length_b                   21.351(3)
_cell_length_c                   17.623(2)
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      23.98
_cell_measurement_theta_min      2.20
_cell_volume                     3859.3(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33524
_diffrn_reflns_theta_full        23.98
_diffrn_reflns_theta_max         23.98
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    1.255
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.6103
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.518
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         6025
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0626P)^2^+5.0217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1109
_reflns_number_gt                4984
_reflns_number_total             6025
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4012058_si_001.cif
_cod_data_source_block           afmii104_0m
_cod_original_cell_volume        3859.4(9)
_cod_database_code               4335421