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_7044265
_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         'C12 H20 O4 Si2'
_chemical_formula_sum            'C12 H20 O4 Si2'
_chemical_formula_weight         284.46
_chemical_name_systematic
2,5-Bis[(trimethylsilyl)oxy]-2,5-cyclohexadiene-1,4-dione
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-15
_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                 100.550(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.38820(16)
_cell_length_b                   9.9721(3)
_cell_length_c                   11.9758(3)
_cell_measurement_reflns_used    1992
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.0870
_cell_measurement_theta_min      5.8010
_cell_volume                     750.01(4)
_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      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    -51.00 -20.00   1.00    1.00    --  -41.65 -37.00 -90.00   31
  2  \w    -99.00 -56.00   1.00    1.00    --  -41.65 -37.00 -90.00   43
  3  \w    -83.00  33.00   1.00    1.00    --  -41.65  19.00 120.00  116
  4  \w     80.00 172.00   1.00    1.00    --  112.00  77.00-150.00   92
  5  \w    140.00 175.00   1.00    1.00    --  112.00 111.00-180.00   35
  6  \w     42.00 138.00   1.00    1.00    --  112.00 -45.00  60.00   96
  7  \w    135.00 178.00   1.00    1.00    --  112.00  45.00  90.00   43
  8  \w     58.00 110.00   1.00    1.00    --  112.00-111.00 -60.00   52
  9  \w     35.00 105.00   1.00    1.00    --  112.00 -94.00 -30.00   70
;
_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      -0.0315574000
_diffrn_orient_matrix_UB_12      0.0966008000
_diffrn_orient_matrix_UB_13      -0.1020329000
_diffrn_orient_matrix_UB_21      0.1770368000
_diffrn_orient_matrix_UB_22      0.0914045000
_diffrn_orient_matrix_UB_23      0.0635647000
_diffrn_orient_matrix_UB_31      0.1670030000
_diffrn_orient_matrix_UB_32      -0.0786942000
_diffrn_orient_matrix_UB_33      -0.0514505000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2455
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.994
_diffrn_reflns_theta_min         5.815
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.199
_exptl_absorpt_correction_T_max  0.867
_exptl_absorpt_correction_T_min  0.555
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       block
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.539
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.077
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         1415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.3273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0834
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1333
_reflns_number_total             1415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02565c2.cif
_cod_data_source_block           3
_cod_original_cell_volume        750.01(3)
_cod_database_code               7044265
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C12H20O4Si2
_reflns_odcompleteness_completeness 99.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              51605
_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 1.330
_oxdiff_exptl_absorpt_empirical_full_min 0.664