Endo- and Exocyclic Supramolecular Complexes of Mixed-Donor Macrocycles via [1:1] and [2:2] Cyclizations
Seul-Gi Lee; Ki-Min Park; Yoichi Habata; Shim Sung Lee; Inorganic Chemistry 52 (2013) 8416–8426; doi:10.1021/ic400247q

data_4335522
_publ_section_title
;
 Endo- and Exocyclic Supramolecular Complexes of Mixed-Donor Macrocycles
 via [1:1] and [2:2] Cyclizations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8416
_journal_page_last               8426
_journal_paper_doi               10.1021/ic400247q
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C50 H54 Cd N6 O10 S4'
_chemical_formula_sum            'C50 H54 Cd N6 O10 S4'
_chemical_formula_weight         1139.63
_chemical_name_systematic
; 
 ? 
;
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_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 90.3050(10)
_cell_angle_gamma                115.7620(10)
_cell_formula_units_Z            2
_cell_length_a                   13.3879(2)
_cell_length_b                   15.2353(3)
_cell_length_c                   15.5975(3)
_cell_measurement_reflns_used    6640
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.38
_cell_measurement_theta_min      2.54
_cell_volume                     2516.40(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0551
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            40839
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_T_max  0.9562
_exptl_absorpt_correction_T_min  0.8909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.129
_refine_diff_density_min         -1.526
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         9900
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0620P)^2^+4.8479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1462
_reflns_number_gt                7175
_reflns_number_total             9900
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400247q_si_002_2.cif
_cod_data_source_block           2
_cod_original_cell_volume        2516.40(8)
_cod_database_code               4335522