1,3-Dinitrone Pincer Complexes of Palladium and Nickel: Synthesis, Structural Characterizations, and Catalysis
Zhang, Yao; Song, Guoyong; Ma, Gaoyuan; Zhao, Jing; Pan, Cheng-Ling; Li, Xingwei; Organometallics 28 (2009) 3233–; doi:10.1021/om900009h

data_4069081
_publ_section_title
;
 1,3-Dinitrone Pincer Complexes of Palladium and Nickel: Synthesis,
 Structural Characterizations, and Catalysis
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              3233
_journal_paper_doi               10.1021/om900009h
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C16 H25 N2 Ni O3, Br, C0.5 H Cl'
_chemical_formula_sum            'C16.5 H26 Br Cl N2 Ni O3'
_chemical_formula_weight         474.46
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 94.205(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.5218(6)
_cell_length_b                   13.2137(5)
_cell_length_c                   20.4587(8)
_cell_measurement_reflns_used    7713
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.19
_cell_measurement_theta_min      2.30
_cell_volume                     4184.8(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            53779
_diffrn_reflns_theta_full        30.56
_diffrn_reflns_theta_max         30.56
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    2.980
_exptl_absorpt_correction_T_max  0.6634
_exptl_absorpt_correction_T_min  0.4891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pyramid
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.915
_refine_diff_density_min         -1.787
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         12729
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0364P)^2^+17.5892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1324
_reflns_number_gt                9607
_reflns_number_total             12729
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900009h_si_003.cif
_cod_data_source_block           lxw40
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C16.50 H26 Br Cl N2 Ni O3'
_cod_database_code               4069081