Developing a "Highway Code" To Steer the Structural and Electronic Properties of Fe(III)/Dy(III) Coordination Clusters.
Chen, Sihuai; Mereacre, Valeriu; Prodius, Denis; Kostakis, George E.; Powell, Annie K.; Inorganic chemistry 54 (2015) 3218–3227; doi:10.1021/ic502809y

data_4342647
_publ_section_title
;
 Developing a &quot;Highway Code&quot; To Steer the Structural and
 Electronic Properties of Fe(III)/Dy(III) Coordination Clusters.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3218
_journal_page_last               3227
_journal_paper_doi               10.1021/ic502809y
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C88 H107 Dy2 Fe4 N4 O26, C2 H3 N'
_chemical_formula_sum            'C90 H110 Dy2 Fe4 N5 O26'
_chemical_formula_weight         2226.22
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-01-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.06 svn.r3119 for OlexSys, GUI svn.r4979)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.001(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3144(16)
_cell_length_b                   29.190(4)
_cell_length_c                   22.497(2)
_cell_measurement_temperature    298
_cell_volume                     9565(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            63992
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.116
_diffrn_reflns_theta_min         1.983
_exptl_absorpt_coefficient_mu    2.208
_exptl_absorpt_correction_T_max  0.6193
_exptl_absorpt_correction_T_min  0.4573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_description       block
_exptl_crystal_F_000             4516
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.043
_refine_diff_density_min         -1.726
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1078
_refine_ls_number_reflns         18799
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      3.737
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0639P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1104
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12273
_reflns_number_total             18799
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502809y_si_001.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4342647--4342650.cif.'
_cod_original_cell_volume        9564.5(19)
_cod_database_code               4342647
_shelxl_version_number           2014-1
_shelx_estimated_absorpt_t_max   0.619
_shelx_estimated_absorpt_t_min   0.457
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C31-C32
 1.53 with sigma of 0.02
 C7-C52 = C30-C31
 1.5 with sigma of 0.02
 C31-C32
 1.5 with sigma of 0.02
 C102-C103
 1.53 with sigma of 0.02
 N6-C102
 1.11 with sigma of 0.02
 O10-C28
 1.43 with sigma of 0.02
3. Rigid bond restraints
 C32, C31, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C103, C102, N6, H10C, H10D, H10E
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C30 \\sim C31 \\sim C32: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C28: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
N6 \\sim C102 \\sim C103 \\sim H10C \\sim H10D \\sim H10E: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C28) = Uanis(C27)
Uanis(C15) = Uanis(C16) = Uanis(C14)
5. Rigid body (RIGU) restrains
 C30, C31, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C103, N6, C102, H10C, H10D, H10E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Riding coordinates:
 O1(H1), O2(H2), C22(H22A,H22B), C23(H23A,H23B), C27(H27A,H27B), C30(H30A,H30B)
6.b Secondary CH2 refined with riding coordinates:
 C0AA(H0AA,H0AB), C1AA(H1AA,H1AB), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B),
  C21(H21A,H21B), C25(H25A,H25B), C26(H26A,H26B), C28(H28A,H28B), C29(H29A,
 H29B), C31(H31A,H31B)
6.c Me refined with riding coordinates:
 C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C24(H24A,H24B,H24C), C32(H32A,H32B,
 H32C), C103(H10C,H10D,H10E)
6.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C12(H12), C20(H20), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39),
 C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C49(H49), C50(H50), C51(H51),
  C52(H52), C53(H53), C58(H58), C59(H59), C60(H60), C56(H56), C57(H57),
 C67(H67), C66(H66), C65(H65), C64(H64), C63(H63), C70(H70), C71(H71), C72(H72),
  C73(H73), C74(H74), C80(H80), C81(H81), C77(H77), C79(H79), C78(H78),
 C85(H85), C84(H84), C88(H88), C87(H87), C86(H86)
6.e Fitted hexagon refined as free rotating group:
 C58(C59,C60,C55,C56,C57), C62(C67,C66,C65,C64,C63), C80(C81,C76,C77,C79,C78),
 C85(C84,C1,C88,C87,C86)
;