Lanthanide-Directed Fabrication of Four Tetranuclear Quadruple Stranded Helicates Showing Magnetic Refrigeration and Slow Magnetic Relaxation.
Mondal, Amit Kumar; Jena, Himanshu Sekhar; Malviya, Amita; Konar, Sanjit; Inorganic chemistry 55 (2016) 5237–5244; doi:10.1021/acs.inorgchem.6b00177

data_4347453
_publ_section_title
;
 Lanthanide-Directed Fabrication of Four Tetranuclear Quadruple Stranded
 Helicates Showing Magnetic Refrigeration and Slow Magnetic Relaxation.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5237
_journal_page_last               5244
_journal_paper_doi               10.1021/acs.inorgchem.6b00177
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         '(C88 H88 Dy4 N16 O26), 2(C2 H3 O2), 5(O H2)'
_chemical_formula_sum            'C92 H104 Dy4 N16 O35'
_chemical_formula_weight         2633.84
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2015-11-17
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                108.258(5)
_cell_angle_beta                 94.285(5)
_cell_angle_gamma                90.647(5)
_cell_formula_units_Z            2
_cell_length_a                   17.336(3)
_cell_length_b                   17.945(3)
_cell_length_c                   18.528(3)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    106(2)
_cell_measurement_theta_max      26.21
_cell_measurement_theta_min      2.31
_cell_volume                     5454.8(16)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      105.7
_diffrn_measured_fraction_theta_full 0.9955
_diffrn_measured_fraction_theta_max 0.9955
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            232351
_diffrn_reflns_theta_full        26.2558
_diffrn_reflns_theta_max         26.26
_diffrn_reflns_theta_min         2.25
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.793
_exptl_absorpt_correction_T_max  0.497
_exptl_absorpt_correction_T_min  0.322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1169 before and 0.0693 after correction.
The Ratio of minimum to maximum transmission is 0.8790.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.6035
_exptl_crystal_description       block
_exptl_crystal_F_000             2604.5360
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
 ?
;
_refine_diff_density_max         3.3281
_refine_diff_density_min         -3.6176
_refine_diff_density_rms         0.3108
_refine_ls_d_res_high            0.8033
_refine_ls_d_res_low             9.0399
_refine_ls_goodness_of_fit_ref   1.0951
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_constraints    170
_refine_ls_number_parameters     1279
_refine_ls_number_reflns         21950
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0951
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0882
_refine_ls_shift/su_max          0.0376
_refine_ls_shift/su_mean         0.0412
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0168P)^2^+227.4920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1964
_refine_ls_wR_factor_ref         0.2176
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              21
_reflns_limit_h_min              -21
_reflns_limit_k_max              21
_reflns_limit_k_min              -22
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                18494
_reflns_number_total             21950
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ic6b00177_si_002.cif
_cod_data_source_block           2
_cod_original_cell_volume        5454.8(15)
_cod_database_code               4347453
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C79) = Uanis(C30)
Uanis(C73) = Uanis(C14)
Uanis(C48) = Uanis(C25)
Uanis(C66) = Uanis(C61)
Uanis(N9) = Uanis(N10)
Uanis(N8) = Uanis(N15)
Uanis(C49) = Uanis(C11)
Uanis(O15) = Uanis(C79)
Uanis(C54) = Uanis(C87)
Uanis(C31) = Uanis(C32)
Uanis(O2) = Uanis(C43)
Uanis(C30) = Uanis(C30a)
Uanis(C79) = Uanis(C79a)
3. Others
 Sof(C30a)=Sof(C79a)=1-FVAR(1)
 Sof(C30)=Sof(C79)=FVAR(1)
 Fixed Sof: O0aa(0.5) O0aa(0.25) O0aa(0.5) O2aa(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C19(H19a,H19b), C21(H21a,H21b), C34(H34a,H34b), C36(H36a,H36b), C37(H37a,
 H37b), C41(H41a,H41b), C51(H51a,H51b), C58(H58a,H58b), C61(H61a,H61b),
 C66(H66a,H66b), C67(H67a,H67b), C80(H80a,H80b), C87(H87a,H87b), C89(H89a,H89b)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20),
 C22(H22), C25(H25), C26(H26), C39(H39), C42(H42), C44(H44), C46(H46), C47(H47),
  C48(H48), C55(H55), C59(H59), C64(H64), C70(H70), C71(H71), C73(H73),
 C78(H78), C81(H81), C82(H82), C86(H86), C90(H90), C91(H91), C92(H92), N1(H1),
 N5(H5), N7(H7), N8(H8), N10(H10), N12(H12a), N16(H16a), C85(H85), C6(H6)
4.c Idealised Me refined as rotating group:
 C28(H28a,H28b,H28c), C31(H31a,H31b,H31c), C32(H32a,H32b,H32c), C33(H33a,H33b,
 H33c), C52(H52a,H52b,H52c), C54(H54a,H54b,H54c), C56(H56a,H56b,H56c), C74(H74a,
 H74b,H74c), C76(H76a,H76b,H76c)
;
_olex2_submission_special_instructions 'No special instructions were received'