Syntheses, structures, luminescence and magnetic properties of three high-nuclearity neodymium compounds based on mixed sulfonylcalix[4]arene-phosphonate ligands
Su, Kongzhao; Jiang, Feilong; Wu, Mingyan; Qian, Jinjie; Pang, Jiandong; Yuan, Daqiang; Hong, Maochun; CrystEngComm 18 (2016) 4921–; doi:10.1039/C6CE00092D

data_7224470
_publ_section_title
;
 Syntheses, structures, luminescence and magnetic properties of three
 high-nuclearity neodymium compounds based on mixed
 sulfonylcalix[4]arene-phosphonate ligands
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              4921
_journal_paper_doi               10.1039/C6CE00092D
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C326 H491 N23 Nd19 O159 P5 S20'
_chemical_formula_weight         10813.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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
_audit_update_record
;
2016-02-23 deposited with the CCDC.
2016-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                72.9520(10)
_cell_angle_beta                 75.9180(10)
_cell_angle_gamma                63.911(2)
_cell_formula_units_Z            2
_cell_length_a                   23.9081(4)
_cell_length_b                   26.1353(5)
_cell_length_c                   43.1391(5)
_cell_measurement_reflns_used    48521
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.5080
_cell_measurement_theta_min      3.1820
_cell_volume                     22938.8(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_sigmaI/netI    0.0951
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            167307
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         70.00
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    17.786
_exptl_absorpt_correction_T_max  0.2058
_exptl_absorpt_correction_T_min  0.1420
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10830
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
SQUEEZE removed 11 DMF and 14 CH3OH molecules per formula unit. 
This valueis calculated based upon volume/count_electrons analysis 
together with element 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         2.291
_refine_diff_density_min         -1.467
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3989
_refine_ls_number_reflns         85093
_refine_ls_number_restraints     359
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0940P)^2^+36.4875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1810
_refine_ls_wR_factor_ref         0.1996
_reflns_number_gt                52754
_reflns_number_total             85093
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce00092d2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7224468--7224470.cif.'
_cod_original_cell_volume        22938.8(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7224470