Variable coordination behaviour of pyrazole-containing N,P and N,P(O) ligands towards palladium(II).
Kealey, Steven; Long, Nicholas J.; Miller, Philip W.; White, Andrew J. P.; Hitchcock, Peter B.; Gee, Antony; Dalton transactions (Cambridge, England : 2003)  (2007) 2823–2832; doi:10.1039/b704051b

data_7005661
_publ_section_title
;
 Variable coordination behaviour of pyrazole-containing N,P and N,P(O)
 ligands towards palladium(II).
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2823
_journal_page_last               2832
_journal_paper_doi               10.1039/b704051b
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C42 H34 N4 O2 P2 Pd, 4(C H Cl3), 2(Cl O4)'
_chemical_formula_sum            'C46 H38 Cl14 N4 O10 P2 Pd'
_chemical_formula_weight         1471.44
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2006-09-04T09:33:38-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.343(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.5748(3)
_cell_length_b                   19.1391(7)
_cell_length_c                   17.7847(6)
_cell_measurement_reflns_used    10936
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     2917.92(18)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.112973
_diffrn_orient_matrix_UB_12      0.64765E-2
_diffrn_orient_matrix_UB_13      0.134312E-1
_diffrn_orient_matrix_UB_21      -0.223792E-1
_diffrn_orient_matrix_UB_22      0.483047E-1
_diffrn_orient_matrix_UB_23      0.182666E-1
_diffrn_orient_matrix_UB_31      -0.185503E-1
_diffrn_orient_matrix_UB_32      -0.188329E-1
_diffrn_orient_matrix_UB_33      0.514711E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17925
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         3.41
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.071
_exptl_absorpt_correction_T_max  0.9756
_exptl_absorpt_correction_T_min  0.9003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.194
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         5693
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+8.7488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1576
_reflns_number_gt                3921
_reflns_number_total             5693
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b704051b.txt
_cod_data_source_block           (2c)-sep206
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7005661