Coordination Studies of a New Unsymmetrical κ4-PNN'N''-Tetradentate Ligand: Stepwise Formation and Structural Characterization
Sean E. Durran; Mark R. J. Elsegood; Shelly R. Hammond; Martin B. Smith; Inorganic Chemistry 46 (2007) 2755–2766; doi:10.1021/ic061196s

data_4306916
_publ_section_title
;
Coordination Studies of a New Unsymmetrical
\k4-PNN'N''-Tetradentate Ligand: Stepwise Formation and
Structural Characterization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2755
_journal_page_last               2766
_journal_paper_doi               10.1021/ic061196s
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C35 H30 Cl2 N3 O3 P Pt'
_chemical_formula_weight         837.58
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   'geom except H2 & H3 coords freely refined'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.757(2)
_cell_angle_beta                 107.033(2)
_cell_angle_gamma                90.723(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2631(4)
_cell_length_b                   12.6371(5)
_cell_length_c                   13.9101(5)
_cell_measurement_reflns_used    11031
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.01
_cell_measurement_theta_min      2.54
_cell_volume                     1621.93(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_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 0.994
_diffrn_measured_fraction_theta_max 0.875
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0137
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14573
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.01
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.580
_exptl_absorpt_correction_T_max  0.657
_exptl_absorpt_correction_T_min  0.406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03, Sheldrick, G.M., (2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         7543
_refine_ls_number_restraints     265
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0173
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0153P)^2^+1.0648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0377
_refine_ls_wR_factor_ref         0.0390
_reflns_number_gt                6999
_reflns_number_total             7543
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic061196ssi20060703_115123_3.cif
_cod_data_source_block           4a
_cod_database_code               4306916