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_7042771
_publ_section_title
;
 Metallocyclic Ni4Ln2M2 single-molecule magnets
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00948H
_journal_year                    2017
_chemical_formula_moiety
'C96 H96 Co2 Dy2 N20 Ni4 O18, 2(C3 H7 N O), 8(O), 2(C2 H3 N), 4(C2 N)'
_chemical_formula_sum            'C114 H148 Co2 Dy2 N28 Ni4 O28'
_chemical_formula_weight         3036.30
_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   geom
_audit_creation_date             2016-08-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-03-13 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.17(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.883(3)
_cell_length_b                   22.825(5)
_cell_length_c                   18.842(4)
_cell_measurement_reflns_used    27953
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      31.5074
_cell_measurement_theta_min      2.0655
_cell_volume                     7040(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      153.15
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0624
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            81133
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.462
_diffrn_reflns_theta_min         1.705
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    1.874
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8429
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3100
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.26
_refine_diff_density_max         2.753
_refine_diff_density_min         -3.355
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     870
_refine_ls_number_reflns         23188
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0726
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0802P)^2^+17.7491P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1833
_refine_ls_wR_factor_ref         0.1952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19955
_reflns_number_total             23188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00948h2.cif
_cod_data_source_block           3
_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               7042771
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C55-C54 = C55-C54A
 1.5 with sigma of 0.01
 C54-N13 = C54A-N13A
 1.15 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(N13A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C52A)=Sof(N12A)=1-FVAR(1)
 Sof(C52)=Sof(N12)=FVAR(1)
 Sof(C54A)=Sof(N13A)=1-FVAR(2)
 Sof(C54)=Sof(N13)=FVAR(2)
 Fixed Sof: N14(0.5) C56(0.5) C57(0.5) H57A(0.5) H57B(0.5) H57C(0.5) C58(0.5)
 H58A(0.5) H58B(0.5) H58C(0.5) C59(0.5) N15(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C26(H26A,H26B), C43(H43A,H43B), C44(H44A,H44B)
5.b 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.c 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.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C41(H41A,H41B,H41C), C58(H58A,H58B,H58C)
;
_shelx_res_checksum              84095
_olex2_submission_special_instructions 'No special instructions were received'