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_4335524
_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 H56 N6 Ni O10 S4'
_chemical_formula_sum            'C50 H56 N6 Ni O10 S4'
_chemical_formula_weight         1087.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.529(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.6383(13)
_cell_length_b                   11.9057(14)
_cell_length_c                   19.717(2)
_cell_measurement_reflns_used    1575
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.51
_cell_measurement_theta_min      2.29
_cell_volume                     2481.1(5)
_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  0.0952
_diffrn_reflns_av_sigmaI/netI    0.0808
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21053
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  0.9127
_exptl_absorpt_correction_T_min  0.8666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       block
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.249
_refine_diff_density_min         -1.147
_refine_diff_density_rms         0.099
_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     322
_refine_ls_number_reflns         4871
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1361
_refine_ls_R_factor_gt           0.0771
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1099P)^2^+3.9336P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1971
_refine_ls_wR_factor_ref         0.2339
_reflns_number_gt                2822
_reflns_number_total             4871
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400247q_si_002_4.cif
_cod_data_source_block           4
_cod_database_code               4335524