Self-assembly of two high-nuclearity manganese calixarene-phosphonate clusters: diamond-Like Mn16 and drum-Like Mn14
Su, Kongzhao; Jiang, Feilong; Qian, Jinjie; Pan, Jie; Pang, Jiandong; Wan, Xiuyan; Hu, Falu; Hong, Maochun; RSC Adv.  (2015) –; doi:10.1039/C5RA02530C

data_7220040
_publ_section_title
;
 Self-assembly of two high-nuclearity manganese calixarene-phosphonate
 clusters: diamond-Like Mn16 and drum-Like Mn14
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA02530C
_journal_year                    2015
_chemical_formula_sum            'C166 H89 Cl Mn16 N0 O69 P8 S12'
_chemical_formula_weight         4809.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-02-03 deposited with the CCDC.
2015-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   34.378(4)
_cell_length_b                   28.140(4)
_cell_length_c                   22.849(3)
_cell_measurement_temperature    293(2)
_cell_volume                     22104(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            144413
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    1.139
_exptl_absorpt_correction_T_max  0.8043
_exptl_absorpt_correction_T_min  0.7639
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9764
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
SQUEEZE removed 18 CH3OH molecules per formula unit. 
This valueis calculated based upon volume/count_electrons analysis.
See ref: a) Y. F. Bi, X. T. Wang, W. P. Liao, X. F. Wang, X. W. Wang,
H. J. Zhang and S. Gao, J. Am. Chem. Soc. 2009, 131, 11650;
b)Y. F. Bi, S. C. Du and W. P. Liao, Chem. Commun., 2011, 47, 4724.
;
_refine_diff_density_max         1.334
_refine_diff_density_min         -1.109
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1331
_refine_ls_number_reflns         20856
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0709
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1274P)^2^+29.5901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1987
_refine_ls_wR_factor_ref         0.2137
_reflns_number_gt                16959
_reflns_number_total             20856
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra02530c2.cif
_cod_data_source_block           d:2
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7220040