Synthesis and Diastereoselectiveortho-Lithiation/Cyclopalladation of Enantiopure [2-Imidazolyl]-1‘,2‘,3‘,4‘,5‘-pentamethylferrocenes and -1‘,2‘,3‘,4‘,5‘-pentaphenylferrocenes
Peters, René; Xin, Zhuo-qun; Fischer, Daniel F.; Schweizer, W. Bernd; Organometallics 25 (2006) 2917–; doi:10.1021/om060187o

data_4075290
_publ_section_title
;
 Synthesis and Diastereoselectiveortho-Lithiation/Cyclopalladation of
 Enantiopure
 [2-Imidazolyl]-1&#x2018;,2&#x2018;,3&#x2018;,4&#x2018;,5&#x2018;-pentamethylferrocenes
 and
 -1&#x2018;,2&#x2018;,3&#x2018;,4&#x2018;,5&#x2018;-pentaphenylferrocenes
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2917
_journal_paper_doi               10.1021/om060187o
_journal_volume                  25
_journal_year                    2006
_chemical_compound_source        'Peters laboratory'
_chemical_formula_moiety         'C44 H46 Fe I N2 P Pd '
_chemical_formula_sum            'C44 H46 Fe I N2 P Pd'
_chemical_formula_weight         922.991
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           maXus
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8571(2)
_cell_length_b                   20.2970(4)
_cell_length_c                   21.4132(4)
_cell_measurement_reflns_used    34896
_cell_measurement_temperature    153
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     3849.51(14)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'SIR97(Cascarano al.,Acta Cryst.,1996,A52,C-79)'
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      -0.05007
_diffrn_orient_matrix_UB_12      -0.07504
_diffrn_orient_matrix_UB_13      -0.06789
_diffrn_orient_matrix_UB_21      0.00704
_diffrn_orient_matrix_UB_22      -0.03521
_diffrn_orient_matrix_UB_23      0.03373
_diffrn_orient_matrix_UB_31      -0.04132
_diffrn_orient_matrix_UB_32      0.01017
_diffrn_orient_matrix_UB_33      0.01923
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            8470
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.00
_exptl_absorpt_coefficient_mu    1.721
_exptl_absorpt_correction_T_max  1.262
_exptl_absorpt_correction_T_min  1.250
_exptl_absorpt_correction_type   cylinder
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cube
_exptl_crystal_size_max          .24
_exptl_crystal_size_mid          .16
_exptl_crystal_size_min          .16
_refine_diff_density_max         1.844
_refine_diff_density_min         -1.451
_refine_diff_density_rms         0.268
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.285
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         8449
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.285
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+ (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1543
_refine_ls_wR_factor_ref         0.1612
_reflns_number_gt                7949
_reflns_number_total             8449
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060187osi20060226_064538.cif
_cod_data_source_block           global
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21 21 21    '
_cod_original_formula_sum        'C44 H46 Fe I N2 P Pd '
_cod_database_code               4075290