Thermal expansion and magnetic properties of benzoquinone-bridged dinuclear rare-earth complexes
Moilanen, Jani; Mansikkamäki, Akseli; Lahtinen, Manu; Guo, Fu-Sheng; Kalenius, Elina; Layfield, Richard; Chibotaru, Liviu F.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02565C

data_7044264
_publ_section_title
;
 Thermal expansion and magnetic properties of benzoquinone-bridged
 dinuclear rare-earth complexes
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02565C
_journal_year                    2017
_chemical_formula_moiety         'C30 H50 Cl4 O10 Y2'
_chemical_formula_sum            'C30 H50 Cl4 O10 Y2'
_chemical_formula_weight         890.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-08-31 deposited with the CCDC.
2017-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.160(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.0004(2)
_cell_length_b                   14.8832(3)
_cell_length_c                   14.8047(3)
_cell_measurement_reflns_used    4260
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      76.6640
_cell_measurement_theta_min      5.9020
_cell_volume                     1904.80(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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     37.00  88.00   1.00    1.85    --   41.65-125.00  60.00   51
  2  \w     44.00 128.00   1.00    7.41    --  112.00 -77.00  30.00   84
  3  \w     30.00 106.00   1.00    7.41    --  112.00 -94.00   0.00   76
  4  \w     24.00  53.00   1.00    1.85    --   41.65-125.00-180.00   29
  5  \w     57.00  98.00   1.00    1.85    --   41.65-125.00-180.00   41
  6  \w     86.00 162.00   1.00    7.41    --  112.00  77.00 -90.00   76
  7  \w    101.00 148.00   1.00    7.41    --  112.00 111.00  90.00   47
  8  \w     79.00 177.00   1.00    7.41    --  112.00  77.00 150.00   98
  9  \w   -115.00 -17.00   1.00    1.85    --  -41.65 -37.00-150.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1707790000
_diffrn_orient_matrix_UB_12      0.0296657000
_diffrn_orient_matrix_UB_13      0.0306342000
_diffrn_orient_matrix_UB_21      0.0418279000
_diffrn_orient_matrix_UB_22      -0.0779569000
_diffrn_orient_matrix_UB_23      -0.0568908000
_diffrn_orient_matrix_UB_31      -0.0290256000
_diffrn_orient_matrix_UB_32      0.0612789000
_diffrn_orient_matrix_UB_33      -0.0869807000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6301
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.981
_diffrn_reflns_theta_min         5.196
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.069
_exptl_absorpt_correction_T_max  0.487
_exptl_absorpt_correction_T_min  0.189
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.148
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3443
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0362P)^2^+0.2319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0764
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3034
_reflns_number_total             3443
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02565c2.cif
_cod_data_source_block           1
_cod_database_code               7044264
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C15H25Cl2Y5O5
_reflns_odcompleteness_completeness 99.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10a,H10b), C12(H12a,H12b), C13(H13a,H13b), C15(H15a,H15b), C16(H16a,
 H16b), C17(H17a,H17b), C19(H19a,H19b), C20(H20a,H20b), C21(H21a,H21b),
 C23(H23a,H23b), C24(H24a,H24b), C26(H26a,H26b)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11)
;
_shelx_res_checksum              72757
_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 1.262
_oxdiff_exptl_absorpt_empirical_full_min 0.872