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_4335042
_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 Mn2 N24 O12 4+], [Cl O4 -1]2, [C2 H3 O2 -1]2'
_chemical_formula_sum            'C120 H94 Cl2 Mn2 N24 O24'
_chemical_formula_weight         2436.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 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                   39.647(5)
_cell_length_b                   15.4126(19)
_cell_length_c                   27.329(3)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.722
_cell_measurement_theta_min      2.156
_cell_volume                     16700(3)
_computing_cell_refinement       'SAINT (Bruker AXS)'
_computing_data_collection       'COSMO (Bruker AXS)'
_computing_data_reduction        'SADABS (Bruker AXS)'
_computing_molecular_graphics    'SHELXL-97, 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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX II DUO'
_diffrn_measurement_method       'phi and 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  0.1028
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            68100
_diffrn_reflns_theta_full        20.82
_diffrn_reflns_theta_max         20.82
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    0.242
_exptl_absorpt_correction_T_max  0.9809
_exptl_absorpt_correction_T_min  0.9332
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.969
_exptl_crystal_description       prism
_exptl_crystal_F_000             5032
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
A significant solvent disorder necessitated solvent flattening
using SQUEEZE. The disordered atoms may comprise acetonitrile solvent,
acetic acid, acetate, or perchlorate ions. In the ordered component, 
one Acetate and one perchlorate ion were found and refined. However,
Ther protonation state of the Acetic acid was not determined, and thus
additional anionic acetate and/or perchlorate may have been SQUEEZed.
PLATON reports that due to low resolution, the electron count may not
be reliable.
;
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.42(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         8776
_refine_ls_number_restraints     335
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0642
_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^)+(0.0941P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.1737
_reflns_number_gt                6194
_reflns_number_total             8776
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4003498_si_002_2.cif
_cod_data_source_block           1
_cod_original_cell_volume        16700(4)
_cod_database_code               4335042