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_7042774
_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 N20 Ni4 O18 Tb2, 2(C3 H7 N O), 13.31(O), 2.69(C2 H3 N)'
_chemical_formula_sum            'C107.38 H148.69 Fe2 N24.69 Ni4 O33.31 Tb2'
_chemical_formula_weight         2982.75
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2017-03-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-03-16 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.51(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.930(3)
_cell_length_b                   22.828(5)
_cell_length_c                   19.005(4)
_cell_measurement_reflns_used    28387
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      31.3889
_cell_measurement_theta_min      2.0626
_cell_volume                     7111(3)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      163.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            55243
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.784
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    1.771
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8161
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3053
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.201
_refine_diff_density_min         -2.801
_refine_diff_density_rms         0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     826
_refine_ls_number_reflns         13916
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0795
_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^)+(0.0696P)^2^+63.8770P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2014
_refine_ls_wR_factor_ref         0.2040
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13253
_reflns_number_total             13916
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00948h2.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/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 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7042774
_shelxl_version_number           2013-2
_olex2_refinement_description
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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
 C53-C54
 1.4 with sigma of 0.01
 C54-N12
 1.15 with sigma of 0.01
 C53-N12
 2.55 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O8W) \\sim Ueq, Uanis(N12) \\sim Ueq, Uanis(N14) \\sim Ueq, Uanis(O3W)
\\sim Ueq, Uanis(O9W) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C56) \\sim Ueq,
Uanis(C57) \\sim Ueq, Uanis(O7WA) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(O7WA)=1-FVAR(1)
 Sof(O7W)=FVAR(1)
 Sof(O9W)=1-FVAR(2)
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C54)=Sof(N12)=FVAR(2)
 Sof(O8W)=1-FVAR(3)
 Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(N14)=Sof(C56)=FVAR(3)
5.a Riding coordinates:
 O1W(H1WA,H1WB)
5.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C26(H26A,H26B), C43(H43A,H43B), C44(H44A,H44B)
5.c Me refined with riding coordinates:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C27(H27A,H27B,H27C), C42(H42A,H42B,
 H42C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C50(H50A,
 H50B,H50C), C57(H57A,H57B,H57C)
5.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C13(H13), C14(H14), C15(H15), C17(H17), C19(H19), C28(H28),
 C30(H30), C31(H31), C33(H33), C34(H34), C36(H36), C37(H37), C39(H39), C40(H40),
  C48(H48), C51(H51)
5.e Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C41(H41A,H41B,H41C), C53(H53A,H53B,H53C)
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_olex2_submission_special_instructions 'No special instructions were received'