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_4335422
_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_moiety         'C32 H58 As N5 Si3 Zr, C2 H5 O0.5'
_chemical_formula_sum            'C34 H63 As N5 O0.5 Si3 Zr'
_chemical_formula_weight         800.30
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.9720(10)
_cell_angle_beta                 72.2780(10)
_cell_angle_gamma                70.5930(10)
_cell_formula_units_Z            2
_cell_length_a                   11.3755(6)
_cell_length_b                   12.1971(6)
_cell_length_c                   16.5256(8)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.59
_cell_volume                     2059.76(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27250
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    1.181
_exptl_absorpt_correction_T_max  0.9166
_exptl_absorpt_correction_T_min  0.7333
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       block
_exptl_crystal_F_000             842
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.102
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         10195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+0.7692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0661
_reflns_number_gt                8808
_reflns_number_total             10195
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4012058_si_002.cif
_cod_data_source_block           rw637zr
_cod_original_sg_symbol_Hall     -P1
_cod_original_formula_sum        'C34 H63 As N5 O0.50 Si3 Zr'
_cod_database_code               4335422