Unusual Metal-Coordinated Zwitterionic P-C-N-C-N-C Phosphido Adducts
Allen T. Ekubo; Mark R. J. Elsegood; Andrew J. Lake; Martin B. Smith; Inorganic Chemistry 49 (2010) 3703–3705; doi:10.1021/ic1002308

data_4315340
_publ_section_title
;
 Unusual Metal-Coordinated Zwitterionic P-C-N-C-N-C Phosphido Adducts
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3703
_journal_page_last               3705
_journal_paper_doi               10.1021/ic1002308
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         '(C34 H34 N4 P2 F4 Pd2 Cl4)(C2 H6 S O)'
_chemical_formula_sum            'C36 H40 Cl4 F4 N4 O P2 Pd2 S'
_chemical_formula_weight         1069.32
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   'geom except H2 coord freely refined'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.980(3)
_cell_length_b                   19.430(4)
_cell_length_c                   12.751(2)
_cell_measurement_reflns_used    38823
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.03
_cell_measurement_theta_min      2.49
_cell_volume                     4206.8(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6710
_diffrn_reflns_av_R_equivalents  0.0895
_diffrn_reflns_av_sigmaI/netI    0.0575
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36669
_diffrn_reflns_theta_full        26.61
_diffrn_reflns_theta_max         26.61
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    1.287
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2004/1, Sheldrick, G.M., (2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
;
_refine_diff_density_max         2.704
_refine_diff_density_min         -1.178
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         5231
_refine_ls_number_restraints     223
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0913P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1535
_reflns_number_gt                3877
_reflns_number_total             5231
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic1002308_si_002_2.cif
_cod_data_source_block           3
_cod_original_cell_volume        4206.7(14)
_cod_database_code               4315340