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_4335045
_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_formula_moiety         '(C58 H44 N12 O6 0), 4(C H4 O)'
_chemical_formula_sum            'C62 H60 N12 O10'
_chemical_formula_weight         1133.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 106.286(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.0686(13)
_cell_length_b                   17.2120(19)
_cell_length_c                   13.7659(15)
_cell_measurement_reflns_used    9123
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.934
_cell_measurement_theta_min      2.367
_cell_volume                     2744.8(5)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0655
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34484
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.9905
_exptl_absorpt_correction_T_min  0.9538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 35510 Corrected reflections written to file
 Estimated minimum and maximum transmission:  0.6812  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    1.371
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Four identifiable, but badly disordered methanol molecules 
were removed using SQUEEZE. These were included in the atom
formula.Approximate locations are
C1S   1   -0.137650    0.221467    0.229117    11.00000
C2S   1    0.408987    0.365227   -0.198794    11.00000
C3S   1    0.155227    0.199902    0.295406    11.00000
C4S   1    0.712844    0.306118   -0.196821    11.00000
O1S   4   -0.224212    0.274012    0.200243    11.00000
O2S   4    0.324094    0.381264   -0.268844    11.00000
O3S   4    0.124010    0.232548    0.210431    11.00000
O4S   4    0.682075    0.379599   -0.218534    11.00000
;
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2.6(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         12226
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1365
_reflns_number_gt                7405
_reflns_number_total             12226
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4003498_si_002_5.cif
_cod_data_source_block           L'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4335045