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_7000346
_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         'C54 H60 N O4 P, C H2 Cl2'
_chemical_formula_sum            'C55 H62 Cl2 N O4 P'
_chemical_formula_weight         902.93
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                65.8298(3)
_cell_angle_beta                 77.0409(3)
_cell_angle_gamma                76.6873(3)
_cell_formula_units_Z            4
_cell_length_a                   13.2138(1)
_cell_length_b                   19.6378(1)
_cell_length_c                   22.6813(2)
_cell_measurement_reflns_used    147382
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_volume                     5169.01(7)
_computing_cell_refinement       HKL2000
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'HKL2000, SortAV, SQUEEZE'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            102943
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    0.200
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.15
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1207
_refine_ls_number_reflns         23594
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0491P)^2^+1.6491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1090
_reflns_number_gt                19081
_reflns_number_total             23594
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b814469a.txt
_cod_data_source_block           s3382a
_cod_database_code               7000346