Chiral Nickel(II) and Palladium(II) NCN-Pincer Complexes Based on Substituted Benzene: Synthesis, Structure, and Lewis Acidity
Bugarin, Alejandro; Connell, Brian T.; Organometallics 27 (2008) 4357–; doi:10.1021/om8004367

data_4071869
_publ_section_title
;
 Chiral Nickel(II) and Palladium(II) NCN-Pincer Complexes Based on
 Substituted Benzene: Synthesis, Structure, and Lewis Acidity
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4357
_journal_paper_doi               10.1021/om8004367
_journal_volume                  27
_journal_year                    2008
_chemical_absolute_configuration rm
_chemical_formula_sum            'C30 H31 Br N2 O2 Pd'
_chemical_formula_weight         637.88
_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_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                   6.6808(7)
_cell_length_b                   19.625(2)
_cell_length_c                   20.422(2)
_cell_measurement_reflns_used    939
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      60.86
_cell_measurement_theta_min      3.12
_cell_volume                     2677.5(5)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_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      110(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'MWPC area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_sigmaI/netI    0.0584
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19307
_diffrn_reflns_theta_full        59.99
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         4.33
_exptl_absorpt_coefficient_mu    7.570
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.5182
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'yellow    '
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'needle    '
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.414
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         3920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+5.2564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1121
_reflns_number_gt                3494
_reflns_number_total             3920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8004367_si_002.cif
_cod_data_source_block           G
_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_cell_volume        2677.6(5)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4071869