Positional disorder manifested as compositional in a pseudo-<i>C</i>~2~-symmetrical Pd complex
Guzei, Ilia A.; Spencer, Lara C.; Ojwach, Stephen O.; Darkwa, James; Acta Crystallographica Section C 64 (2008) m114–m116; doi:10.1107/S0108270108002503

data_2016513
_publ_section_title
;
 Positional disorder manifested as compositional in a
 pseudo-<i>C</i>~2~-symmetrical Pd complex
;
_journal_coeditor_code           SK3199
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m114
_journal_page_last               m116
_journal_paper_doi               10.1107/S0108270108002503
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Pd (C18 H18 F6 N5)] (C32 H12 B F24)'
_chemical_formula_moiety         'C18 H18 F6 N5 Pd +, C32 H12 B F24 -'
_chemical_formula_sum            'C50 H30 B F30 N5 Pd'
_chemical_formula_weight         1388.00
_chemical_name_systematic
;{2-[3,5-bis(trifluoromethyl)-1H-pyrazol-1-ylmethyl]-6-(3,5-dimethyl-1H-pyrazol-
1-ylmethyl)pyridine}methylpalladium(II)
tetrakis[3,5-bis(trifluoromethyl)phenyl]borate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 96.8650(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9194(4)
_cell_length_b                   18.0256(7)
_cell_length_c                   27.1635(11)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      29.14
_cell_measurement_theta_min      1.89
_cell_volume                     5308.2(4)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008), publCIF (Westrip, 2008) and
modiCIFer (Guzei, 2007)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      105(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_diffrn_measurement_method       '0.30\% \w '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            92342
_diffrn_reflns_theta_full        29.14
_diffrn_reflns_theta_max         29.14
_diffrn_reflns_theta_min         1.89
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.498
_exptl_absorpt_correction_T_max  0.8815
_exptl_absorpt_correction_T_min  0.8412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2007)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.26
_refine_diff_density_max         2.160
_refine_diff_density_min         -1.628
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         14211
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+17.6386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1544
_reflns_number_gt                12423
_reflns_number_total             14211
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3199.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2016513
_cod_database_fobs_code          2016513