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_4342648
_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         'C128 H156 Dy4 Fe4 N4 O36, C2 H3 N'
_chemical_formula_sum            'C130 H159 Dy4 Fe4 N5 O36'
_chemical_formula_weight         3241.01
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                89.624(6)
_cell_angle_beta                 87.037(6)
_cell_angle_gamma                73.680(6)
_cell_formula_units_Z            2
_cell_length_a                   14.0948(11)
_cell_length_b                   16.8520(13)
_cell_length_c                   29.6754(19)
_cell_measurement_temperature    180
_cell_volume                     6755.4(9)
_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      180
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.982
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_av_unetI/netI     0.0859
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            40487
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.359
_diffrn_reflns_theta_min         1.374
_exptl_absorpt_coefficient_mu    2.677
_exptl_absorpt_correction_T_max  0.6165
_exptl_absorpt_correction_T_min  0.5006
_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    1.593
_exptl_crystal_description       block
_exptl_crystal_F_000             3260
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.654
_refine_diff_density_min         -1.823
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1501
_refine_ls_number_reflns         24304
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.900
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1017P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1530
_refine_ls_wR_factor_ref         0.1684
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14489
_reflns_number_total             24304
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502809y_si_001.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4342647--4342650.cif.'
_cod_database_code               4342648
_shelxl_version_number           2014-1
_shelx_estimated_absorpt_t_max   0.617
_shelx_estimated_absorpt_t_min   0.501
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H13C,H13D,H13E} of C131, {H18C,H18D,H18E} of C181, {H12C,
  H12D,H12E} of C121, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  {H24A,H24B,H24C} of C24, {H32A,H32B,H32C} of C32, {H40A,H40B,H40C} of C40,
  {H48A,H48B,H48C} of C48, {H57A,H57B,H57C} of C57, {H16A,H16B,H16C} of C16,
  {H81A,H81B,H81C} of C81, {H97A,H97B,H97C} of C97, {H10C,H10D,H10E} of C105,
  {H89A,H89B,H89C} of C89, {H73A,H73B,H73C} of C73, {H65A,H65B,H65C} of C65,
  {H8A,H8B,H8C} of C8, {H12F,H12G,H12H} of C129, {H11C,H11D,H11E} of C113
2. Restrained distances
 N0AA-C130
 1.1 with sigma of 0.02
 C130-C131
 1.5 with sigma of 0.02
 C117-C121 = C177-C181
 1.51 with sigma of 0.02
 O1-H1 = O2-H2 = O3-H3 = O4-H4
 0.88 with sigma of 0.04
3. Rigid bond restraints
 C115, C116, C117, C118, C119, C120, C121
 with sigma for 1-2 distances of 0.04 and sigma for 1-3 distances of 0.08
 C175, C176, C177, C178, C179, C180, C181
 with sigma for 1-2 distances of 0.04 and sigma for 1-3 distances of 0.08
4. Uiso/Uaniso restraints and constraints
: with sigma of 0.08 and sigma for terminal atoms of 0.15
: with sigma of 0.08 and sigma for terminal atoms of 0.14
Uiso(C115) = Uiso(C175)
Uiso(C116) = Uiso(C176)
Uiso(C117) = Uiso(C177)
Uiso(C118) = Uiso(C178)
Uiso(C119) = Uiso(C179)
Uiso(C120) = Uiso(C180)
Uiso(C121) = Uiso(C181)
Uanis(C84) = Uanis(C85) = Uanis(C86) = Uanis(C87) = Uanis(C88) = Uanis(C83) =
Uanis(C89)
Uanis(C60) = Uanis(C59) = Uanis(C64) = Uanis(C63) = Uanis(C62) = Uanis(C61) =
Uanis(C65)
5. Others
 Fixed Sof: C115(0.5) C116(0.5) H116(0.5) C117(0.5) C118(0.5) H118(0.5)
 C119(0.5) H119(0.5) C120(0.5) H120(0.5) C175(0.5) C176(0.5) H176(0.5)
 C177(0.5) C178(0.5) H178(0.5) C179(0.5) H179(0.5) C180(0.5) H180(0.5)
 C121(0.5) H12C(0.5) H12D(0.5) H12E(0.5) C181(0.5) H18C(0.5) H18D(0.5) H18E(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C0AA(H0AA,H0AB), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B),
 C1AA(H1AA,H1AB), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C17(H17A,H17B),
  C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,
 H22B), C23(H23A,H23B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B),
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B)
6.b Me refined with riding coordinates:
 C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C24(H24A,H24B,H24C), C32(H32A,H32B,
 H32C), C40(H40A,H40B,H40C), C48(H48A,H48B,H48C), C57(H57A,H57B,H57C), C65(H65A,
 H65B,H65C), C73(H73A,H73B,H73C), C81(H81A,H81B,H81C), C97(H97A,H97B,H97C),
 C105(H10C,H10D,H10E), C113(H11C,H11D,H11E), C121(H12C,H12D,H12E), C181(H18C,
 H18D,H18E), C129(H12F,H12G,H12H)
6.c Aromatic/amide H refined with riding coordinates:
 C35(H35), C37(H37), C38(H38), C39(H39), C43(H43), C44(H44), C45(H45),
 C47(H47), C52(H52), C53(H53), C54(H54), C56(H56), C60(H60), C62(H62), C63(H63),
  C64(H64), C68(H68), C70(H70), C71(H71), C72(H72), C76(H76), C78(H78),
 C79(H79), C80(H80), C84(H84), C85(H85), C86(H86), C88(H88), C92(H92), C94(H94),
  C95(H95), C96(H96), C100(H100), C102(H102), C103(H103), C104(H104),
 C108(H108), C110(H110), C111(H111), C112(H112), C116(H116), C118(H118),
 C119(H119), C120(H120), C176(H176), C178(H178), C179(H179), C180(H180),
 C124(H124), C126(H126), C127(H127), C128(H128)
6.d Fitted hexagon refined as free rotating group:
 C115(C116,C117,C118,C119,C120), C175(C176,C177,C178,C179,C180)
6.e Idealised Me refined as rotating group:
 C89(H89A,H89B,H89C), C131(H13C,H13D,H13E)
;
_olex2_submission_special_instructions 'No special instructions were received'