Synthesis of bis[palladium(II)] and bis[platinum(II)] complexes containing chiral, linear quadridentate ligands with a P2N2 donor set
Justine Bennett; A. David Rae; Geoffrey Salem; Natalie C. Ward; Paul Waring; Kerri Wells; Anthony C. Willis; J. Chem. Soc., Dalton Trans.  (2002) 234–243; doi:10.1039/b106861j

data_7011026
_publ_section_title
;
 Synthesis of bis[palladium(II)] and bis[platinum(II)] complexes
 containing chiral, linear quadridentate ligands with a P2N2 donor set
;
_journal_issue                   2
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              234
_journal_page_last               243
_journal_paper_doi               10.1039/b106861j
_journal_year                    2002
_chemical_formula_moiety
'C47 H56 N4 P2 Pd2 2+, 0.5(Cl -), 1.5( F6 P -), 1.5(C3 H6 O) '
_chemical_formula_sum            'C51.5 H65 Cl0.5 F9 N4 O1.5 P3.5 Pd2'
_chemical_formula_weight         1274.07
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      18
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_audit_creation_date             1999-10-19
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
2001-07-31  passes checkcif with warnings - see refine_special_details
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.622(4)
_cell_length_b                   21.207(3)
_cell_length_c                   16.001(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193.2
_cell_measurement_theta_max      51.5
_cell_measurement_theta_min      46.5
_cell_volume                     5980(2)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1994)
;
_diffrn_ambient_temperature      193.2
_diffrn_measurement_device_details
;
Rigaku AFC6R diffractometer with extended arm and
evacuated collimator and beam tunnel.
Data cannot be collected beyond \y 60 deg in this configuration.
;
_diffrn_measurement_device_type  'Rigaku AFC6R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.03378
_diffrn_orient_matrix_UB_12      0.02923
_diffrn_orient_matrix_UB_13      0.03195
_diffrn_orient_matrix_UB_21      -0.02436
_diffrn_orient_matrix_UB_22      0.03693
_diffrn_orient_matrix_UB_23      -0.02812
_diffrn_orient_matrix_UB_31      -0.03855
_diffrn_orient_matrix_UB_32      0.00228
_diffrn_orient_matrix_UB_33      0.04576
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.06617
_diffrn_reflns_av_sigmaI/netI    0.070
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9587
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         60.11
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        1.48
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.51
_exptl_absorpt_correction_T_max  .458
_exptl_absorpt_correction_T_min  .256
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.0
_refine_diff_density_min         -0.8
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.396
_refine_ls_goodness_of_fit_ref   1.463
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     260
_refine_ls_number_reflns         7442
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.076
_refine_ls_R_factor_gt           0.060
_refine_ls_shift/su_max          0.3
_refine_ls_shift/su_mean         0.1
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.0025|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.096
_refine_ls_wR_factor_ref         0.093
_reflns_number_gt                7442
_reflns_number_total             8883
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            b106861j.txt
_cod_data_source_block           ncw2
_cod_original_cell_volume        5980(3)
_cod_original_sg_symbol_H-M      'P 21 21 2  '
_cod_original_formula_sum        'C51.5 H65 Cl0.5 F9 N4 O1.5 P3.5 Pd2 '
_cod_database_code               7011026