Formation of Molecular Ladder Elements with Macrocyclic Platforms via Linear Bifunctional Ligands
Wei Huang; Shaohua Gou; Dahua Hu; Suchada Chantrapromma; Hoong-Kun Fun; Qingjin Meng; Inorganic Chemistry 41 (2002) 864–868; doi:10.1021/ic010407k

data_4317541
_publ_section_title
;
 Formation of Molecular Ladder Elements with Macrocyclic Platforms via
 Linear Bifunctional Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              864
_journal_page_last               868
_journal_paper_doi               10.1021/ic010407k
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C63 H69 Cl2 N11 O18 Zn4'
_chemical_formula_weight         1600.67
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                66.9563(8)
_cell_angle_beta                 80.5638(8)
_cell_angle_gamma                76.6348(8)
_cell_formula_units_Z            1
_cell_length_a                   11.6520(3)
_cell_length_b                   12.1394(3)
_cell_length_c                   13.8462(3)
_cell_measurement_reflns_used    7449
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.48
_cell_measurement_theta_min      1.60
_cell_volume                     1747.52(7)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material
;
SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990)
;
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.865
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_device_type
;
Siemens SMART CCD area detector diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_sigmaI/netI    0.1031
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12808
_diffrn_reflns_theta_full        29.53
_diffrn_reflns_theta_max         29.53
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    1.509
_exptl_absorpt_correction_T_max  0.5836
_exptl_absorpt_correction_T_min  0.5437
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.985
_refine_diff_density_min         -1.126
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.0101(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         8441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0748P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1487
_refine_ls_wR_factor_ref         0.1619
_reflns_number_gt                5203
_reflns_number_total             8441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic010407k_2.cif
_cod_data_source_block           hwa126m
_cod_database_code               4317541