Unique 2:1 Complex with a trans-Chelating Bis-Pyridine Ligand
Yi-Zhen Hu; Charles Chamchoumis; Janusz S. Grebowicz; Randolph P. Thummel; Inorganic Chemistry 41 (2002) 2296–2300; doi:10.1021/ic010965z

data_4317856
_publ_section_title
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 Unique 2:1 Complex with a trans-Chelating Bis-Pyridine Ligand
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2296
_journal_page_last               2300
_journal_paper_doi               10.1021/ic010965z
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C40 H24 N4 Pd 2+, 2 B F4 -, 1.5 H2 O'
_chemical_formula_sum            'C40 H27 B2 F8 N4 O1.5 Pd'
_chemical_formula_weight         867.68
_chemical_name_systematic
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   ?
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_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'I -2ya'
_symmetry_space_group_name_H-M   'I 1 a 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                 112.105(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.8098(12)
_cell_length_b                   12.1354(6)
_cell_length_c                   28.9445(15)
_cell_measurement_reflns_used    5371
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      23.50
_cell_measurement_theta_min      1.52
_cell_volume                     7423.1(7)
_computing_cell_refinement       'Bruker SAINT software (Bruker, 1999)'
_computing_data_collection       'Siemens SMART software (Siemens, 1996)'
_computing_data_reduction        'Bruker SAINT software (Bruker, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 1K
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       CCD
_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  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            17206
_diffrn_reflns_theta_full        23.50
_diffrn_reflns_theta_max         23.50
_diffrn_reflns_theta_min         1.52
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.581
_exptl_absorpt_correction_T_max  0.8917
_exptl_absorpt_correction_T_min  0.8353
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Prismatic block'
_exptl_crystal_F_000             3480
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.32(3)
_refine_ls_extinction_coef       0.00003(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     916
_refine_ls_number_reflns         10242
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.687
_refine_ls_shift/su_mean         0.095
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+18.3726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.1047
_reflns_number_gt                8395
_reflns_number_total             10772
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            ic010965z.cif
_cod_data_source_block           k604
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_original_formula_sum        'C40 H27 B2 N4 O1.5 F8 Pd'
_cod_database_code               4317856