Self-Assembly of the First Discrete 3d‒4f‒4f Triple-Stranded Helicate
Riis-Johannessen, Thomas; Bernardinelli, Gérald; Filinchuk, Yaroslav; Clifford, Sarah; Dalla Favera, Natalia; Piguet, Claude; Inorganic Chemistry 48 (2009) 5512–5525; doi:10.1021/ic900654m

data_4302403
_publ_section_title
;
 Self-Assembly of the First Discrete 3d--4f--4f Triple-Stranded Helicate
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5512
_journal_page_last               5525
_journal_paper_doi               10.1021/ic900654m
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C173 H150 F24 Lu2 N36 O27 S8 Zn'
_chemical_formula_weight         4293.08
_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                90.679(4)
_cell_angle_beta                 93.321(4)
_cell_angle_gamma                117.501(4)
_cell_formula_units_Z            2
_cell_length_a                   15.8708(8)
_cell_length_b                   16.0222(5)
_cell_length_c                   47.308(2)
_cell_measurement_temperature    100(1)
_cell_volume                     10642.4(9)
_computing_cell_refinement       'CrysAlis (Oxford Diffraction, 2006)'
_computing_data_collection       'MAR345 control software (MAR, 2002)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction, 2006)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  'SHELXTL (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL (Bruker, 2001)'
_computing_structure_solution    'SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'MAR345 Image plate'
_diffrn_measurement_method       \f-scan
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_source         'Beamline BM1A, SNBL, ESRF, Grenoble, France'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.72242
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_av_sigmaI/netI    0.0720
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            42023
_diffrn_reflns_theta_full        20.48
_diffrn_reflns_theta_max         20.48
_diffrn_reflns_theta_min         1.92
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.199
_exptl_absorpt_correction_T_max  0.732
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4344
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.244
_refine_diff_density_min         -2.144
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.721
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     937
_refine_ls_number_reflns         18528
_refine_ls_number_restraints     813
_refine_ls_restrained_S_all      1.689
_refine_ls_R_factor_all          0.1779
_refine_ls_R_factor_gt           0.1517
_refine_ls_shift/su_max          0.656
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4149
_refine_ls_wR_factor_ref         0.4495
_reflns_number_gt                12257
_reflns_number_total             18528
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4338553
_cod_data_source_file            ic900654m_si_002.cif
_cod_data_source_block           squeezed
_cod_original_cell_volume        10642.3(8)
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               4302403