Architectural Spiroligomers Designed for Binuclear Metal Complex Templating
Shivaiah Vaddypally; Chongsong Xu; Senzhi Zhao; Yanfeng Fan; Christian E. Schafmeister; Michael J. Zdilla; Inorganic Chemistry 52 (2013) 6457–6463; doi:10.1021/ic4003498

data_4335043
_publ_section_title
;
 Architectural Spiroligomers Designed for Binuclear Metal Complex
 Templating
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6457
_journal_page_last               6463
_journal_paper_doi               10.1021/ic4003498
_journal_volume                  52
_journal_year                    2013
_chemical_absolute_configuration syn
_chemical_formula_moiety         '(C116 H88 N24 O12 Zn2 4+), (Cl O4 1-)4'
_chemical_formula_sum            'C116 H88 Cl4 N24 O28 Zn2'
_chemical_formula_weight         2538.64
_space_group_IT_number           1
_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                88.0000(10)
_cell_angle_beta                 72.1180(10)
_cell_angle_gamma                67.7800(10)
_cell_formula_units_Z            1
_cell_length_a                   13.9716(11)
_cell_length_b                   16.1139(13)
_cell_length_c                   19.7129(16)
_cell_measurement_reflns_used    9046
_cell_measurement_temperature    172(2)
_cell_measurement_theta_max      27.940
_cell_measurement_theta_min      2.426
_cell_volume                     3893.4(5)
_computing_cell_refinement       'SAINT (Bruker AXS)'
_computing_data_collection       'COSMO (Bruker AXS)'
_computing_data_reduction        'SADABS (Bruker AXS)'
_computing_molecular_graphics    'XP (Sheldrick, 1997)'
_computing_publication_material  'APEX2 (Bruker AXS)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      172(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker KAPPA APEX II DUO'
_diffrn_measurement_method       'phi/omega 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  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            58201
_diffrn_reflns_theta_full        27.95
_diffrn_reflns_theta_max         27.95
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.442
_exptl_absorpt_correction_T_max  0.9655
_exptl_absorpt_correction_T_min  0.7188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
58201 Corrected reflections written to file 
 Estimated minimum and maximum transmission:  0.6861  0.7456
 The ratio of these values is more reliable than their absolute values!
 Additional spherical absorption correction applied with mu*r =  0.2000
 Lambda/2 correction factor = 0.0015
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_description       plate
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.08
_platon_squeeze_details
; Disordered solvent in the cavities was removed using SQUEEZE. 
This removed 428 electrons from a 10 voids with a total volume
of 1436.5 angstroms. This is consistent with the removal of between
8 and 20 molecules of acetonitrile, acetic acid, and/or toluene. 
This corresponds to 50-60 atoms, which is consistent with the void
size.
;
_refine_diff_density_max         0.753
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.219(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1495
_refine_ls_number_reflns         33334
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0553
_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^)+(0.0970P)^2^+1.1396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1722
_reflns_number_gt                26055
_reflns_number_total             33334
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4003498_si_002_3.cif
_cod_data_source_block           2
_cod_database_code               4335043