Diimine supported group 10 hydroxo, oxo, amido, and imido complexes
Singh, Anupam; Anandhi, U.; Cinellu, Maria Agostina; Sharp, Paul R.; Dalton Transactions  (2008) 2314–2327; doi:10.1039/b715663d

data_7003347
_publ_section_title
;
 Diimine supported group 10 hydroxo, oxo, amido, and imido complexes
;
_journal_issue                   17
_journal_name_full               'Dalton Transactions'
_journal_page_first              2314
_journal_page_last               2327
_journal_paper_doi               10.1039/b715663d
_journal_year                    2008
_chemical_formula_moiety         'C50 H64 N6 Pd2 2+, 2(B F4 1-), 4(C H2 Cl2)'
_chemical_formula_sum            'C54 H72 B2 Cl8 F8 N6 Pd2'
_chemical_formula_weight         1475.20
_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                 77.461(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.627(4)
_cell_length_b                   24.551(8)
_cell_length_c                   11.490(4)
_cell_measurement_reflns_used    946
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      2.80
_cell_volume                     3201.6(19)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics
;
L. J. Barbour, X-Seed - Graphical Interface to
SHELX-97 and POV-Ray, 1999
ORTEP (Johnson, 1976), ORTEP 3 for Windows (L. J. Farrugia, 1997)
;
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement
;
SHELXL-97 (Sheldrick, 1997), L. J. Barbour, X-Seed - Graphical Interface to
SHELX-97 and POV-Ray, 1999
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19471
_diffrn_reflns_theta_full        27.17
_diffrn_reflns_theta_max         27.17
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.959
_exptl_absorpt_correction_T_max  0.9102
_exptl_absorpt_correction_T_min  0.6456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Data were corrected for decay and absorption using the program SADABS
based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995).
;
_exptl_crystal_colour            orange-yellow
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.304
_refine_diff_density_min         -1.272
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         7033
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+5.5886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1070
_reflns_number_gt                5786
_reflns_number_total             7033
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715663d.txt
_cod_data_source_block           Pd2(NHtol)2(bpy)2(BF4)2_(12,Ar=tol)
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3201.8(17)
_cod_original_sg_symbol_H-M      'P2(1)/c '
_cod_database_code               7003347