Ring Methyl Activation of 1,2-Dimethyl-3,4-di(tert-butyl)cyclobutadiene Complexes of Palladium Givingexo-Methylene-η3-cyclobutenyl Complexes of Palladium
Mashima, Kazushi; Shimizu, Daisuke; Yamagata, Tsuneaki; Tani, Kazuhide; Organometallics 21 (2002) 5136–; doi:10.1021/om0204484

data_4077034
_publ_section_title
;
 Ring Methyl Activation of 1,2-Dimethyl-3,4-di(tert-butyl)cyclobutadiene
 Complexes of Palladium Givingexo-Methylene-\h3-cyclobutenyl Complexes of
 Palladium
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5136
_journal_paper_doi               10.1021/om0204484
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C19 H30 Cl3 N Pd'
_chemical_formula_weight         485.19
_chemical_melting_point          471.5(15)
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'Apr 12 10:12:11 1999'
_audit_update_record             'May 27 21:15:00 2002'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.587(3)
_cell_length_b                   16.097(3)
_cell_length_c                   10.841(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      14.94
_cell_measurement_theta_min      14.57
_cell_volume                     2196.5(9)
_computing_cell_refinement       'Rigaku/RAPID Diffractometer Control'
_computing_data_collection       'Rigaku/RAPID Diffractometer Control'
_computing_data_reduction        'teXsan: PROCESS (MSC)'
_computing_molecular_graphics    'Ortep-3 (Louis J. Farrugia, 1999)'
_computing_publication_material  'SHELXL-97 and modified'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1999)'
_computing_structure_solution    'SIR97(A. Altomare, et al., 1999)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  AFC7R
_diffrn_measurement_method       \w-2\t
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2866
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        2.96
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.211
_exptl_absorpt_correction_T_max  0.7032
_exptl_absorpt_correction_T_min  0.7651
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
'( North, Phillips, & Mathews, (1968). Acta Cryst. A24, 351-359.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2845
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0350P)^2^+2.7182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0855
_reflns_number_gt                2332
_reflns_number_total             2845
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0204484.cif
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '470-473' was changed to '471.5(15)'
- 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_Hall     'P 2AC 2AB'
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               4077034
_diffrn_standards_interval       150