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_7224469
_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            'C215 H309 Cl3 N19 Nd11 O81 P6 S12'
_chemical_formula_weight         6719.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90.00
_cell_angle_beta                 105.7980(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.1600(2)
_cell_length_b                   39.5294(4)
_cell_length_c                   32.4297(3)
_cell_measurement_reflns_used    29203
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.2450
_cell_measurement_theta_min      3.5890
_cell_volume                     27334.5(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0781
_diffrn_reflns_av_sigmaI/netI    0.1037
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            101255
_diffrn_reflns_theta_full        68.00
_diffrn_reflns_theta_max         68.00
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    17.763
_exptl_absorpt_correction_T_max  0.1758
_exptl_absorpt_correction_T_min  0.1253
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             13492
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
SQUEEZE removed 3 DMF and 2 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         4.143
_refine_diff_density_min         -4.276
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2907
_refine_ls_number_reflns         49683
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0842P)^2^+63.0810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1667
_refine_ls_wR_factor_ref         0.1790
_reflns_number_gt                37320
_reflns_number_total             49683
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce00092d2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7224468--7224470.cif.'
_cod_original_cell_volume        27334.5(4)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7224469