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_4335044
_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 Mn N12 O12 +2], [Cl O4 -1]4, 1.5 [C7 H8]
;
_chemical_formula_sum            'C126.5 H100 Cl4 Mn2 N24 O28'
_chemical_formula_weight         2655.99
_chemical_name_systematic
; 
 ? 
;
_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                100.71(3)
_cell_angle_beta                 93.73(3)
_cell_angle_gamma                98.49(3)
_cell_formula_units_Z            2
_cell_length_a                   16.467(3)
_cell_length_b                   24.962(5)
_cell_length_c                   27.659(6)
_cell_measurement_reflns_used    1832
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.533
_cell_measurement_theta_min      2.522
_cell_volume                     10999(4)
_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      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.1322
_diffrn_reflns_av_sigmaI/netI    0.4827
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21428
_diffrn_reflns_theta_full        17.61
_diffrn_reflns_theta_max         17.61
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_T_max  0.9968
_exptl_absorpt_correction_T_min  0.9724
_exptl_absorpt_process_details
;
 21428 Corrected reflections written to file 
 Estimated minimum and maximum transmission:  0.5743  0.7441
 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            colourless
_exptl_crystal_density_diffrn    0.802
_exptl_crystal_description       needle
_exptl_crystal_F_000             2738
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
The structure was SQUEEZED using PLATON, and refined against the corrected
hkl file to remove severely disordered solvent or anion electron density.
;
_refine_diff_density_max         1.123
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.23(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.788
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1038
_refine_ls_number_reflns         18163
_refine_ls_number_restraints     957
_refine_ls_restrained_S_all      0.778
_refine_ls_R_factor_all          0.2299
_refine_ls_R_factor_gt           0.1263
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1070P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2750
_refine_ls_wR_factor_ref         0.3188
_reflns_number_gt                4257
_reflns_number_total             18163
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4003498_si_002_4.cif
_cod_data_source_block           1a
_cod_original_formula_sum        'C126.50 H100 Cl4 Mn2 N24 O28'
_cod_database_code               4335044