Heterometallic CuII/DyIII 1D chiral polymers: chirogenesis and exchange coupling of toroidal moments in trinuclear Dy3 single molecule magnets
Novitchi, Ghenadie; Pilet, Guillaume; Ungur, Liviu; Moshchalkov, Victor V.; Wernsdorfer, Wolfgang; Chibotaru, Liviu F.; Luneau, Dominique; Powell, Annie K.; Chemical Science 3 (2012) 1169–; doi:10.1039/c2sc00728b

data_1515041
_publ_section_title
;
 Heterometallic CuII/DyIII 1D chiral polymers: chirogenesis and exchange
 coupling of toroidal moments in trinuclear Dy3 single molecule magnets
;
_journal_issue                   4
_journal_name_full               'Chemical Science'
_journal_page_first              1169
_journal_paper_doi               10.1039/c2sc00728b
_journal_volume                  3
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C69 H93 Cu2 Gd6 N11 O54'
_chemical_formula_sum            'C69 H93 Cu2 Gd6 N11 O54'
_chemical_formula_weight         3011.14
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-10-15
_audit_creation_method           CRYSTALS_ver_14.11
_cell_angle_alpha                90.0
_cell_angle_beta                 102.060(9)
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   11.3478(13)
_cell_length_b                   24.0164(16)
_cell_length_c                   20.6607(17)
_cell_measurement_reflns_used    10645
_cell_measurement_temperature    110
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     5506.5(9)
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29242
_diffrn_reflns_theta_full        26.178
_diffrn_reflns_theta_max         29.413
_diffrn_reflns_theta_min         3.442
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.029
_exptl_absorpt_correction_T_max  0.46
_exptl_absorpt_correction_T_min  0.28
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2916
_exptl_crystal_size_max          0.396
_exptl_crystal_size_mid          0.306
_exptl_crystal_size_min          0.192
_refine_diff_density_max         1.86
_refine_diff_density_min         -1.58
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.97(2)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0001
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1202
_refine_ls_number_reflns         15094
_refine_ls_number_restraints     162
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0697
_refine_ls_shift/su_max          0.0018399
_refine_ls_shift/su_mean         0.0000300
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
40.2 -33.3 29.9
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0866
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0695
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              25
_reflns_limit_k_min              -33
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                17016
_reflns_number_total             21476
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.96
_oxford_diffrn_Wilson_scale      0.49
_oxford_refine_ls_r_factor_ref   0.0639
_oxford_refine_ls_scale          1.492(2)
_oxford_reflns_number_all        21436
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c2sc00728b.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        5506.5(8)
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_database_code               1515041
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
CONT ENANTIO
RIDE C ( 1,X'S) H ( 11,X'S) H ( 13,X'S) H ( 12,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 5,X'S) H ( 51,X'S)
RIDE C ( 6,X'S) H ( 61,X'S)
RIDE C ( 10,X'S) H ( 101,X'S)
RIDE C ( 21,X'S) H ( 212,X'S) H ( 211,X'S) H ( 213,X'S)
RIDE C ( 24,X'S) H ( 241,X'S)
RIDE C ( 25,X'S) H ( 251,X'S)
RIDE C ( 26,X'S) H ( 261,X'S)
RIDE C ( 30,X'S) H ( 301,X'S)
RIDE C ( 41,X'S) H ( 413,X'S) H ( 411,X'S) H ( 412,X'S)
RIDE C ( 44,X'S) H ( 441,X'S)
RIDE C ( 45,X'S) H ( 451,X'S)
RIDE C ( 46,X'S) H ( 461,X'S)
RIDE C ( 50,X'S) H ( 501,X'S)
RIDE O ( 101,X'S) H (1011,X'S)
RIDE O ( 102,X'S) H (1021,X'S)
RIDE C ( 114,X'S) H (1141,X'S)
RIDE C ( 115,X'S) H (1151,X'S)
RIDE C ( 116,X'S) H (1161,X'S) H (1163,X'S) H (1162,X'S)
RIDE C ( 117,X'S) H (1172,X'S) H (1171,X'S) H (1173,X'S)
RIDE C ( 124,X'S) H (1241,X'S)
RIDE C ( 125,X'S) H (1251,X'S)
RIDE C ( 126,X'S) H (1262,X'S) H (1261,X'S) H (1263,X'S)
RIDE C ( 127,X'S) H (1272,X'S) H (1273,X'S) H (1271,X'S)
RIDE O ( 131,X'S) H (1313,X'S)
RIDE C ( 132,X'S) H (1321,X'S) H (1322,X'S) H (1323,X'S)
RIDE C ( 201,X'S) H (2011,X'S) H (2012,X'S) H (2013,X'S)
RIDE C ( 204,X'S) H (2041,X'S)
RIDE C ( 205,X'S) H (2051,X'S)
RIDE C ( 206,X'S) H (2061,X'S)
RIDE C ( 210,X'S) H (2101,X'S)
RIDE C ( 221,X'S) H (2212,X'S) H (2213,X'S) H (2211,X'S)
RIDE C ( 224,X'S) H (2241,X'S)
RIDE C ( 225,X'S) H (2251,X'S)
RIDE C ( 226,X'S) H (2261,X'S)
RIDE C ( 230,X'S) H (2301,X'S)
RIDE C ( 241,X'S) H (2411,X'S) H (2413,X'S) H (2412,X'S)
RIDE C ( 244,X'S) H (2441,X'S)
RIDE C ( 245,X'S) H (2451,X'S)
RIDE C ( 246,X'S) H (2461,X'S)
RIDE C ( 250,X'S) H (2501,X'S)
RIDE O ( 291,X'S) H (2911,X'S)
RIDE O ( 301,X'S) H (3011,X'S)
RIDE O ( 302,X'S) H (3021,X'S)
RIDE C ( 314,X'S) H (3141,X'S)
RIDE C ( 315,X'S) H (3151,X'S)
RIDE C ( 316,X'S) H (3161,X'S) H (3163,X'S) H (3162,X'S)
RIDE C ( 317,X'S) H (3172,X'S) H (3171,X'S) H (3173,X'S)
RIDE C ( 324,X'S) H (3241,X'S)
RIDE C ( 325,X'S) H (3251,X'S)
RIDE C ( 326,X'S) H (3262,X'S) H (3261,X'S) H (3263,X'S)
RIDE C ( 327,X'S) H (3272,X'S) H (3273,X'S) H (3271,X'S)
RIDE O ( 331,X'S) H (3311,X'S) H (3312,X'S)
EQUIV C(7,U'S) UNTIL C(8)
EQUIV C(27,U'S) UNTIL C(28)
EQUIV C(48,U'S) UNTIL O(49)
EQUIV C(201,U'S) UNTIL O(202)
EQUIV N(281,U'S) UNTIL O(284)
EQUIV N(328,U'S) UNTIL O(331)
END
;
_iucr_refine_instruction_details_restraints
;
NO
DISTANCE 1.250000 , 0.020000 = N(281) TO O(282)
DISTANCE 1.250000 , 0.020000 = N(281) TO O(283)
DISTANCE 1.250000 , 0.020000 = N(281) TO O(284)
DISTANCE 1.400000 , 0.020000 = C(201) TO O(202)
DISTANCE 1.450000 , 0.020000 = C(125) TO C(127)
PLANAR 0.010000 N(281) O(282) O(283) O(284)
ANGLE 120.000000 , 0.500000 = O(282) TO N(281) TO O(283)
ANGLE 120.000000 , 0.500000 = O(282) TO N(281) TO O(284)
U(IJ)'S 0.0, 0.010000 = C(21) TO O(22)
U(IJ)'S 0.0, 0.010000 = C(24) TO C(25)
U(IJ)'S 0.0, 0.010000 = C(41) TO O(42)
U(IJ)'S 0.0, 0.010000 = O(42) TO C(43)
U(IJ)'S 0.0, 0.010000 = C(43) TO C(44)
U(IJ)'S 0.0, 0.010000 = C(44) TO C(45)
U(IJ)'S 0.0, 0.010000 = C(45) TO C(46)
U(IJ)'S 0.0, 0.010000 = C(46) TO C(47)
U(IJ)'S 0.0, 0.010000 = C(50) TO O(51)
U(IJ)'S 0.0, 0.010000 = C(124) TO C(125)
U(IJ)'S 0.0, 0.010000 = C(125) TO C(126)
U(IJ)'S 0.0, 0.010000 = C(126) TO C(127)
U(IJ)'S 0.0, 0.010000 = O(202) TO C(203)
U(IJ)'S 0.0, 0.010000 = C(204) TO C(205)
U(IJ)'S 0.0, 0.010000 = O(209) TO C(210)
U(IJ)'S 0.0, 0.010000 = C(210) TO O(211)
U(IJ)'S 0.0, 0.010000 = C(221) TO O(222)
U(IJ)'S 0.0, 0.010000 = O(222) TO C(223)
U(IJ)'S 0.0, 0.010000 = C(224) TO C(225)
U(IJ)'S 0.0, 0.010000 = N(261) TO O(262)
U(IJ)'S 0.0, 0.010000 = O(284) TO O(291)
U(IJ)'S 0.0, 0.010000 = O(321) TO C(322)
U(IJ)'S 0.0, 0.010000 = GD(13) TO O(282)
U(IJ)'S 0.0, 0.010000 = GD(13) TO O(202)
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
U(IJ)'S 0.0, 0.010000 = GD(2) TO O(51)
END
;