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_7042769
_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 H100 Cr2 N20 Ni4 O18 Y2, 4(C3 H7 N O), 2(C2 H3 N), 6(H2 O), 2(O)'
_chemical_formula_sum            'C112 H150 Cr2 N26 Ni4 O30 Y2'
_chemical_formula_weight         2857.23
_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     heavy
_audit_creation_date             2017-04-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-04-14 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.6390(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.6402(3)
_cell_length_b                   22.7099(3)
_cell_length_c                   19.1594(3)
_cell_measurement_reflns_used    14205
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.3070
_cell_measurement_theta_min      4.5330
_cell_volume                     6972.2(2)
_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 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      1.00  81.00   1.00    1.16    --   40.81 -99.00 -90.00   80
  2  \w     30.00 105.00   1.00    7.00    --  112.00 -95.00 -60.00   75
  3  \w     49.00 102.00   1.00    7.00    --  112.00 -95.00  30.00   53
  4  \w     62.00 140.00   1.00    7.00    --  112.00 -77.00 120.00   78
  5  \w    105.00 177.00   1.00    7.00    --  112.00  30.00  60.00   72
  6  \w    104.00 163.00   1.00    7.00    --  112.00  45.00   0.00   59
  7  \w     83.00 171.00   1.00    7.00    --  112.00  61.00  90.00   88
  8  \w     75.00 116.00   1.00    1.16    --   40.81  77.00  30.00   41
  9  \w     35.00  82.00   1.00    7.00    --  112.00 -95.00 120.00   47
 10  \w      2.00  81.00   1.00    1.16    --   40.81 -99.00 150.00   79
 11  \w   -104.00 -18.00   1.00    1.16    --  -40.81 -38.00 -90.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0468690000
_diffrn_orient_matrix_UB_12      -0.0590176000
_diffrn_orient_matrix_UB_13      -0.0165509000
_diffrn_orient_matrix_UB_21      0.0685897000
_diffrn_orient_matrix_UB_22      -0.0300365000
_diffrn_orient_matrix_UB_23      0.0597937000
_diffrn_orient_matrix_UB_31      -0.0484278000
_diffrn_orient_matrix_UB_32      0.0145889000
_diffrn_orient_matrix_UB_33      0.0559243000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27805
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.991
_diffrn_reflns_theta_min         3.684
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.500
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72317
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       block
_exptl_crystal_F_000             2964
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.187
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         12429
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0927P)^2^+20.8478P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1761
_refine_ls_wR_factor_ref         0.1843
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10339
_reflns_number_total             12429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00948h2.cif
_cod_data_source_block           8
_cod_original_cell_volume        6972.22(19)
_cod_database_code               7042769
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         CHNONiYCr
_chemical_oxdiff_usercomment     CHNONiYCr
_shelx_estimated_absorpt_t_max   0.541
_shelx_estimated_absorpt_t_min   0.420
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H2WA,H2WB} of O2W, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H4WA,H4WB} of O4W, {H5WA,H5WB} of O5W, {H1WA,H1WB} of
  O1W
2. Restrained distances
 O9-C57 = O11-C58
 1.25 with sigma of 0.01
 C57-N13 = C58-N14
 1.3 with sigma of 0.01
 N13-C55 = N13-C56 = N14-C59 = N14-C60
 1.45 with sigma of 0.01
 O9-N13 = O11-N14
 2.26 with sigma of 0.01
 C57-C55 = C57-C56 = C58-C59 = C58-C60
 2.4 with sigma of 0.01
3. Restrained planarity
 O9, C57, N13, C55, C56
 with sigma of 0.1
 O11, C58, N14, C59, C60
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C58) \\sim Ueq, Uanis(N12) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(O11)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. Others
 Sof(N14)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=Sof(C60)=Sof(H60A)=Sof(H60B)=
 Sof(H60C)=Sof(C58)=Sof(H58)=Sof(O11)=1-FVAR(1)
 Sof(O9)=Sof(N13)=Sof(C57)=Sof(H57)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=
 Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=FVAR(1)
6.a Riding coordinates:
 O2W(H2WA,H2WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB)
6.b Rotating group:
 O1W(H1WA,H1WB)
6.c Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C20(H20A,H20B), C37(H37A,H37B), C41(H41A,H41B)
6.d Aromatic/amide H refined with riding coordinates:
 C33(H33), C45(H45), C21(H21), C31(H31), C9(H9), C11(H11), C42(H42), C10(H10),
 C15(H15), C36(H36), C25(H25), C46(H46), C44(H44), C50(H50), C32(H32), C23(H23),
  C24(H24), C57(H57), C58(H58)
6.e Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C48(H48A,H48B,H48C), C29(H29A,H29B,H29C), C7(H7A,H7B,
 H7C), C54(H54A,H54B,H54C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C18(H18A,
 H18B,H18C), C19(H19A,H19B,H19C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C),
 C56(H56A,H56B,H56C), C55(H55A,H55B,H55C), C59(H59A,H59B,H59C), C60(H60A,H60B,
 H60C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.523
_oxdiff_exptl_absorpt_empirical_full_min 0.492