As‒As Bond Formation via Reductive Elimination from a Zirconocene Bis(dimesitylarsenide) Compound
Elrod, L. Taylor; Boxwala, Hussain; Haq, Hira; Zhao, Annie W.; Waterman, Rory; Organometallics 31 (2012) 5204–; doi:10.1021/om300415q

data_4078782
_publ_section_title
;
 As--As Bond Formation via Reductive Elimination from a Zirconocene
 Bis(dimesitylarsenide) Compound
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              5204
_journal_paper_doi               10.1021/om300415q
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C46 H54 As2 Zr'
_chemical_formula_weight         847.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           34
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 -2n'
_symmetry_space_group_name_H-M   'P n n 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.9687(18)
_cell_length_b                   22.0733(19)
_cell_length_c                   9.3097(8)
_cell_measurement_reflns_used    9777
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.37
_cell_volume                     4309.0(6)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            40600
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    1.819
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6333
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.375
_exptl_crystal_size_min          0.338
_platon_squeeze_details
;
The unit cell contained one pentane (or diethylether) molecule that has been treated as a diffuse contribution to the overall scatting without using specific atom positions by the SQUEEZE function in the PLATON program (Spek, 2003). 
;
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.014(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7616
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0306P)^2^+1.8009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0639
_reflns_number_gt                7134
_reflns_number_total             7616
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300415q_si_003.cif
_cod_data_source_block           lte002_0l
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      Pnn2
_cod_database_code               4078782