Two 3d-4f double helical chains including [Dy2M2]n (M = Ni(II) and Co(II)) cores exhibiting slow magnetic relaxation.
She, Shixiong; Li, Yahong; Li, Wu; Dalton transactions (Cambridge, England : 2003) 45 (2016) 10830–10835; doi:10.1039/c6dt00951d

data_7039485
_publ_section_title
;
 Two 3d-4f double helical chains including [Dy2M2]n (M = Ni(II) and
 Co(II)) cores exhibiting slow magnetic relaxation.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10830
_journal_page_last               10835
_journal_paper_doi               10.1039/c6dt00951d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'C60 H50 Co2 Dy2 N5 O22, C62 H51 Co2 Dy2 N5 O23, N O3,12(H2O),2(C2H5OH)'
_chemical_formula_sum            'C126 H137 Co4 Dy4 N11 O62'
_chemical_formula_weight         3683.18
_space_group_crystal_system      tetragonal
_space_group_IT_number           80
_space_group_name_Hall           'I 4bw'
_space_group_name_H-M_alt        'I 41'
_symmetry_space_group_name_Hall  'I 4bw'
_symmetry_space_group_name_H-M   'I 41'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-06-03
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-06-03 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.2860(12)
_cell_length_b                   26.2860(12)
_cell_length_c                   44.3921(15)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      25.242
_cell_measurement_theta_min      0.9
_cell_volume                     30673(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      291.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  MoK\a
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            112866
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.308
_diffrn_reflns_theta_min         0.900
_exptl_absorpt_coefficient_mu    2.436
_exptl_absorpt_correction_T_max  0.614
_exptl_absorpt_correction_T_min  0.563
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       block
_exptl_crystal_F_000             14704
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.400(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.866
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1753
_refine_ls_number_reflns         37997
_refine_ls_number_restraints     2131
_refine_ls_restrained_S_all      0.854
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0222
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0097P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0452
_refine_ls_wR_factor_ref         0.0467
_reflns_Friedel_coverage         0.975
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                29600
_reflns_number_total             37997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00951d2.cif
_cod_data_source_block           2_sq_s
_cod_depositor_comments
'Adding full bibliography for 7039485--7039486.cif.'
_cod_original_cell_volume        30673(3)
_cod_database_code               7039485
_shelx_estimated_absorpt_t_max   0.641
_shelx_estimated_absorpt_t_min   0.592
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.600(4) 0.400(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Restrained distances
 O3-N1 \\sim O2-N1 \\sim O4-N1
 with sigma of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O1(0.5) O5AA(0.5) O6AA(0.5) N1AA(0.5) N1(0.5) O2(0.5) O3(0.5)
 O4(0.5)
6.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB)
6.b Aromatic/amide H refined with riding coordinates:
 C5AA(H5AA), C6AA(H6AA), C5(H5), C8(H8), C10(H10), C0AA(H0AA), C12(H12),
 C13(H13), C18(H18), C19(H19), C20(H20), C23(H23), C25(H25), C26(H26), C27(H27),
  C28(H28), C33(H33), C34(H34), C35(H35), C38(H38), C40(H40), C41(H41),
 C42(H42), C43(H43), C48(H48), C49(H49), C50(H50), C53(H53), C55(H55), C56(H56),
  C57(H57), C58(H58), C63(H63), C64(H64), C65(H65), C68(H68), C70(H70),
 C71(H71), C72(H72), C73(H73), C78(H78), C79(H79), C80(H80), C83(H83), C85(H85),
  C86(H86), C87(H87), C88(H88), C93(H93), C94(H94), C95(H95), C98(H98),
 C100(H100), C101(H101), C102(H102), C103(H103), C108(H108), C109(H109),
 C110(H110), C113(H113), C115(H115), C116(H116), C117(H117), C118(H118)
6.c Idealised Me refined as rotating group:
 C3AA(H3AA,H3AB,H3AC), C16(H16A,H16B,H16C), C31(H31A,H31B,H31C), C1AA(H1AA,
 H1AB,H1AC), C61(H61A,H61B,H61C), C76(H76A,H76B,H76C), C91(H91A,H91B,H91C),
 C106(H10A,H10B,H10C), C122(H12A,H12B,H12C)
;
_shelx_res_checksum              85636
_shelx_fab_checksum              5763
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'