Oxacalix[3]arene-supported supertetrahedron
Stephanie M. Taylor; Ruaraidh D. McIntosh; Julien Reze; Scott J. Dalgarno; Euan K. Brechin; Chemical Communications 48 (2012) 9263–9265; doi:10.1039/c2cc34792j

data_7108319
_publ_section_title
;
 Oxacalix[3]arene-supported supertetrahedron
;
_journal_issue                   74
_journal_name_full               'Chemical Communications'
_journal_page_first              9263
_journal_page_last               9265
_journal_paper_doi               10.1039/c2cc34792j
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C160.5 H225.1 Cl4 Mn10 N5.5 O36.8'
_chemical_formula_weight         3511.56
_chemical_name_common            Mn10Oxa3DMF
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 114.965(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   37.8284(18)
_cell_length_b                   27.8091(13)
_cell_length_c                   37.6849(19)
_cell_measurement_reflns_used    8225
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.52
_cell_measurement_theta_min      2.29
_cell_volume                     35939(3)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'Apex II'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8 Apex II CCD Diffractometer'
_diffrn_measurement_method       '\f and \w 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  0.1410
_diffrn_reflns_av_sigmaI/netI    0.2046
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            133789
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             14712
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.749
_refine_diff_density_min         -1.066
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.236
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1812
_refine_ls_number_reflns         33987
_refine_ls_number_restraints     161
_refine_ls_restrained_S_all      1.244
_refine_ls_R_factor_all          0.2571
_refine_ls_R_factor_gt           0.1056
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2373
_refine_ls_wR_factor_ref         0.2931
_reflns_number_gt                13217
_reflns_number_total             33987
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc34792j.txt
_cod_data_source_block           ST2927
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C160.50 H225.10 Cl4 Mn10 N5.50 O36.80'
_cod_database_code               7108319