A novel hemilabile calix[4],quinoline-based P,N-ligand: coordination chemistry and complex characterisation
Marson, Angelica; Ernsting, Johanneke E.; Lutz, Martin; Spek, Anthony L.; van Leeuwen, Piet W. N. M.; Kamer, Paul C. J.; Dalton Transactions  (2009) 621–; doi:10.1039/b814469a

data_7000347
_publ_section_title
;
 A novel hemilabile calix[4],quinoline-based P,N-ligand: coordination
 chemistry and complex characterisation
;
_journal_issue                   4
_journal_name_full               'Dalton Transactions'
_journal_page_first              621
_journal_paper_doi               10.1039/b814469a
_journal_year                    2009
_chemical_formula_moiety         'C55 H63 Cl N O4 P Pd, 2(C4 H10 O)'
_chemical_formula_sum            'C63 H83 Cl N O6 P Pd'
_chemical_formula_weight         1123.12
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.6368(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.1478(2)
_cell_length_b                   12.93260(10)
_cell_length_c                   18.91510(10)
_cell_measurement_reflns_used    192444
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_volume                     6375.38(8)
_computing_cell_refinement       HKL2000
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'HKL2000, SortAV'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-97 (Beurskens et al., 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            99310
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.06
_platon_squeeze_details          ' ?'
_refine_diff_density_max         1.249
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         14575
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0516P)^2^+2.8673P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1105
_reflns_number_gt                10908
_reflns_number_total             14575
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b814469a.txt
_cod_data_source_block           s3333a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7000347