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_4335041
_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         '[C60 H47 N13 O6] . 0.32 [H2 O]'
_chemical_formula_sum            'C60 H47.64 N13 O6.32'
_chemical_formula_weight         1051.83
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.4132(11)
_cell_length_b                   26.710(5)
_cell_length_c                   30.792(5)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.834
_cell_measurement_theta_min      2.337
_cell_volume                     5274.6(16)
_computing_cell_refinement       'SAINT (Bruker AXS)'
_computing_data_collection       'COSMO (Bruker AXS)'
_computing_data_reduction        'SADABS (Bruker AXS)'
_computing_molecular_graphics    'XP (Sheldrick, 2008)'
_computing_publication_material  'APEX2 (Bruker AXS)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Kappa APEX II DUO'
_diffrn_measurement_method       '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  0.0538
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            35369
_diffrn_reflns_theta_full        20.96
_diffrn_reflns_theta_max         20.96
_diffrn_reflns_theta_min         1.01
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.9947
_exptl_absorpt_correction_T_min  0.9659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
35475 Corrected reflections written to file
 Estimated minimum and maximum transmission:  0.5780  0.7446
 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    1.325
_exptl_crystal_description       needle
_exptl_crystal_F_000             2197
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.1(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     725
_refine_ls_number_reflns         5595
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0460P)^2^+1.3116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0870
_reflns_number_gt                4981
_reflns_number_total             5595
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4003498_si_002_1.cif
_cod_data_source_block           L
_cod_database_code               4335041