Pentanuclear [2.2] spirocyclic lanthanide(iii) complexes: slow magnetic relaxation of the Dy(III) analogue.
Biswas, Sourav; Das, Sourav; van Leusen, Jan; Kögerler, Paul; Chandrasekhar, Vadapalli; Dalton transactions (Cambridge, England : 2003) 44 (2015) 19282–19293; doi:10.1039/c5dt03060a

data_7036810
_publ_section_title
;
 Pentanuclear [2.2] spirocyclic lanthanide(iii) complexes: slow magnetic
 relaxation of the Dy(III) analogue.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19282
_journal_page_last               19293
_journal_paper_doi               10.1039/c5dt03060a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C74 H103 Cl N8 O34.5 Tb5'
_chemical_formula_weight         2486.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-10-27 deposited with the CCDC.
2015-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_formula_units_Z            8
_cell_length_a                   40.479(5)
_cell_length_b                   40.479(5)
_cell_length_c                   11.943(5)
_cell_measurement_reflns_used    9214
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.04
_cell_measurement_theta_min      2.25
_cell_volume                     19569(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'DIAMOND 3.1 d'
_computing_publication_material  'SHELXS-97 (Sheldrick, 1990)'
_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  'Bruker SMART APEX'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1230
_diffrn_reflns_av_sigmaI/netI    0.1132
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            68807
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    3.674
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.4825
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'North et al, 1968'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9768.0
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
;
_refine_diff_density_max         2.419
_refine_diff_density_min         -3.128
_refine_diff_density_rms         0.312
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.002(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1101
_refine_ls_number_reflns         21266
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0802P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1532
_reflns_number_gt                16239
_reflns_number_total             21266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt03060a2.cif
_cod_data_source_block           complex2
_cod_depositor_comments
;
Adding full bibliography for 7036809--7036811.cif.

2018-03-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         4973.50
_cod_original_formula_moiety         'C148 H206 Cl2 N16 O69 Tb10 '
_cod_original_formula_units_Z            4
_cod_original_cell_volume        19569(10)
_cod_original_formula_sum        'C148 H206 Cl2 N16 O69 Tb10 '
_cod_database_code               7036810