Metallocyclic Ni4Ln2M2 single-molecule magnets
Liu, Mei-Jiao; Hu, kong-Qiu; Liu, Cai-Ming; Cui, Ai-Li; Kou, Hui-Zhong; Dalton Trans.  (2017) –; doi:10.1039/C7DT00948H

data_7042772
_publ_section_title
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 Metallocyclic Ni4Ln2M2 single-molecule magnets
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00948H
_journal_year                    2017
_chemical_formula_moiety
'C96 H100 Fe2 Gd2 N20 Ni4 O18, 4(C3 H7 N O), 2(C2 H3 N), 10(H2 O), 4(O)'
_chemical_formula_sum            'C112 H162 Fe2 Gd2 N26 Ni4 O36'
_chemical_formula_weight         3109.64
_chemical_name_systematic
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 ?
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_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             2017-03-04
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
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2017-03-13 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 128.6060(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.0731(2)
_cell_length_b                   15.9253(2)
_cell_length_c                   27.5474(3)
_cell_measurement_reflns_used    19679
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      76.5760
_cell_measurement_theta_min      3.9470
_cell_volume                     6881.56(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ShelXS-98
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            35727
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.998
_diffrn_reflns_theta_min         3.555
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    9.029
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       block
_exptl_crystal_F_000             3191
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.361
_refine_diff_density_min         -1.495
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         12241
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+67.8616P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1686
_refine_ls_wR_factor_ref         0.1701
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11593
_reflns_number_total             12241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00948h2.cif
_cod_data_source_block           7
_cod_original_cell_volume        6881.55(15)
_cod_database_code               7042772
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.777
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O9-C109
 1.25 with sigma of 0.01
 C109-N11
 1.3 with sigma of 0.01
 N11-C107 = N11-C108
 1.45 with sigma of 0.01
 O9-N11
 2.26 with sigma of 0.01
 C109-C108 = C109-C107
 2.4 with sigma of 0.01
3. Restrained planarity
 O9, C109, N11, C108, C107
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(N4) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(C109)
\\sim Ueq, Uanis(O4W) \\sim Ueq, Uanis(O8W) \\sim Ueq, Uanis(N11) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB), O6W(H6WA,
 H6WB), O7W(H7WA,H7WB)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B), C29(H29A,H29B), C31(H31A,H31B)
5.c Me refined with riding coordinates:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C107(H10C,H10D,H10E), C108(H10F,H10G,H10H), C110(H11A,H11B,H11C),
 C112(H11D,H11E,H11F)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C11(H11), C13(H13), C14(H14), C15(H15),
 C24(H24), C25(H25), C26(H26), C28(H28), C32(H32), C34(H34), C35(H35), C36(H36),
  C109(H109), C111(H111)
5.e Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C113(H11G,H11H,H11I)
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_olex2_submission_special_instructions 'No special instructions were received'