Methyl Group Transfer from ZnMe2to Arsenic(III), an Alternative Pathway to Deprotonation of [CyNHAs(μ-NCy)]2
Bond, Andrew D.; Hopkins, Alexander D.; Rothenberger, Alexander; Wolf, Robert; Woods, Anthony D.; Wright, Dominic S.; Organometallics 20 (2001) 4454–; doi:10.1021/om010326w

data_4077355
_publ_section_title
;
 Methyl Group Transfer from ZnMe2to Arsenic(III), an Alternative Pathway
 to Deprotonation of [CyNHAs(\m-NCy)]2
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              4454
_journal_paper_doi               10.1021/om010326w
_journal_volume                  20
_journal_year                    2001
_chemical_formula_moiety         'C28 H58 As2 N4 Zn2'
_chemical_formula_sum            'C28 H58 As2 N4 Zn2'
_chemical_formula_weight         731.36
_chemical_melting_point          430(4)
_chemical_name_systematic
; 
 [{MeAs(NHCy)(NCy)}ZnMe]2 
;
_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                81.031(3)
_cell_angle_beta                 81.754(3)
_cell_angle_gamma                66.919(2)
_cell_formula_units_Z            2
_cell_length_a                   8.1835(5)
_cell_length_b                   9.8676(5)
_cell_length_c                   23.3327(8)
_cell_measurement_reflns_used    12541
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1705.10(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f 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  0.0547
_diffrn_reflns_av_sigmaI/netI    0.0663
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            15944
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.354
_exptl_absorpt_correction_T_max  1.057
_exptl_absorpt_correction_T_min  0.926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav Blessing (1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         7684
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+1.1555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1354
_reflns_number_gt                3349
_reflns_number_total             7684
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om010326w.cif
_cod_data_source_block           dw0115
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '426-433' was changed to '430(4)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077355