Electronic Structures of Bent Lanthanide(III) Complexes with Two N-Donor Ligands
Nicholas, Hannah; Vonci, Michele; Goodwin, Conrad Alexander Phillip; Loo, Song Wei; Murphy, Siobhan; Cassim, Daniel; Winpenny, Richard E. P.; McInnes, Eric J. L.; Chilton, Nicholas F.; Mills, David P.; Chemical Science  (2019) –; doi:10.1039/C9SC03431E

data_1552338
_publ_section_title
;
 Electronic Structures of Bent Lanthanide(III) Complexes with Two N-Donor
 Ligands
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC03431E
_journal_year                    2019
_chemical_formula_moiety         'C36 H84 F N2 Si4 Yb'
_chemical_formula_sum            'C36 H84 F N2 Si4 Yb'
_chemical_formula_weight         849.45
_chemical_name_systematic        '[Yb(Ntt)2(F)]'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-08-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-11-23 deposited with the CCDC.    2019-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                84.182(3)
_cell_angle_beta                 80.590(3)
_cell_angle_gamma                68.517(3)
_cell_formula_units_Z            2
_cell_length_a                   8.7293(3)
_cell_length_b                   11.1712(4)
_cell_length_c                   24.4919(8)
_cell_measurement_reflns_used    12784
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      74.3530
_cell_measurement_theta_min      1.8590
_cell_volume                     2190.30(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.956
_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     70.71 258.71   1.00    8.00    --  100.00  73.87 -55.79  188
  2  \w     70.71 258.71   1.00    8.00    --  100.00  73.87 119.21  188
  3  \f   -171.08  30.04   1.00    8.00 124.98 100.50  73.87    --   201
  4  \w    -46.10 111.90   1.00    5.00    --  -25.00  73.87 164.21  158
  5  \f    -12.99 330.22   1.00    8.00-130.79 111.00  73.87    --   343
  6  \w     72.94 229.94   1.00    5.00    --   75.00  73.87-175.79  157
  7  \w    117.83 225.83   1.00    8.00    --  111.00  73.87  24.21  108
  8  \w    -63.01  48.99   1.00    5.00    --  -35.00  73.87 -65.79  112
  9  \f    167.02 299.18   1.00    8.00 169.21 112.00  73.87    --   132
 10  \f    110.67 210.73   1.00    8.00 159.16 110.00  73.87    --   100
 11  \w    122.67 227.67   1.00    8.00    --  112.00  73.87  -5.79  105
 12  \w     75.90 160.90   1.00    8.00    --  105.00  73.87-110.79   85
 13  \w     27.14 129.11   1.00    5.00    --  -24.50  73.87  61.71  102
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1207372000
_diffrn_orient_matrix_UB_12      0.0008768000
_diffrn_orient_matrix_UB_13      -0.0395451000
_diffrn_orient_matrix_UB_21      0.1231654000
_diffrn_orient_matrix_UB_22      0.0180657000
_diffrn_orient_matrix_UB_23      -0.0499814000
_diffrn_orient_matrix_UB_31      0.0831133000
_diffrn_orient_matrix_UB_32      -0.1472470000
_diffrn_orient_matrix_UB_33      -0.0034594000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            17168
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         1.830
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.206
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       plate
_exptl_crystal_F_000             898
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.487
_refine_diff_density_min         -1.433
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         7685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0598P)^2^+3.1881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7366
_reflns_number_total             7685
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc03431e2.cif
_cod_data_source_block           xdpm73
_cod_original_cell_volume        2190.28(13)
_cod_database_code               1552338
_shelx_shelxl_version_number     2017/1
_reflns_odcompleteness_completeness 90.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     73.97
_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 Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), C10(H10), C13(H13), C16(H16), C19(H19), C22(H22),
 C25(H25), C28(H28), C31(H31), C34(H34)
2.b Idealised Me refined as rotating group:
 C2(H2a,H2b,H2c), C3(H3a,H3b,H3c), C5(H5a,H5b,H5c), C6(H6a,H6b,H6c), C8(H8a,
 H8b,H8c), C9(H9a,H9b,H9c), C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C14(H14a,
 H14b,H14c), C15(H15a,H15b,H15c), C17(H17a,H17b,H17c), C18(H18a,H18b,H18c),
 C20(H20a,H20b,H20c), C21(H21a,H21b,H21c), C23(H23a,H23b,H23c), C24(H24a,H24b,
 H24c), C26(H26a,H26b,H26c), C27(H27a,H27b,H27c), C29(H29a,H29b,H29c), C30(H30a,
 H30b,H30c), C32(H32a,H32b,H32c), C33(H33a,H33b,H33c), C35(H35a,H35b,H35c),
 C36(H36a,H36b,H36c)
;
_shelx_res_checksum              39401
_manchester_internal_archive_date 10/07/2017
_manchester_internal_coll_client FO/CAPG/DP
_manchester_internal_coll_date   10/07/2017
_manchester_internal_coll_frame_method '\w & \f scans'
_manchester_internal_coll_frame_time 5&8s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_name   xdpm73
_manchester_internal_coll_type   custom
_manchester_internal_coll_user   FO
_manchester_internal_process_date 10/07/2017
_manchester_internal_process_user FO
_manchester_internal_refinement_date 10/07/2017
_manchester_internal_refinement_user FO
_manchester_internal_solution_date 10/07/2017
_manchester_internal_solution_user FO
_manchester_internal_validation_date 10/07/2017
_manchester_internal_validation_user FO
_olex2_exptl_crystal_mounting_method 'in fomblin oil on micromount'
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.244
_oxdiff_exptl_absorpt_empirical_full_min 0.440