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_1552336
_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 N2 Si4 Yb, B C24 F20, C H2 Cl2'
_chemical_formula_sum            'C61 H86 B Cl2 F20 N2 Si4 Yb'
_chemical_formula_weight         1594.42
_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
_audit_creation_date             2017-08-24
_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                90
_cell_angle_beta                 92.749(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0620(3)
_cell_length_b                   25.9262(6)
_cell_length_c                   16.7464(3)
_cell_measurement_reflns_used    10054
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      74.6820
_cell_measurement_theta_min      3.1160
_cell_volume                     6965.6(2)
_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)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.979
_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     83.90 269.84   1.00   12.00    --  112.68  73.87-175.79  186
  2  \w     83.90 268.90   1.00   12.00    --  112.68  73.87 -55.79  185
  3  \w    -68.18 116.82   1.00    7.00    --  -39.39  73.87-160.79  185
  4  \w     67.90 254.90   1.00   12.00    --   97.68  73.87  64.21  187
  5  \w      3.12 188.12   1.00    7.00    --   31.90  73.87  76.21  185
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0344668000
_diffrn_orient_matrix_UB_12      -0.0172842000
_diffrn_orient_matrix_UB_13      -0.0799338000
_diffrn_orient_matrix_UB_21      0.0345447000
_diffrn_orient_matrix_UB_22      0.0546178000
_diffrn_orient_matrix_UB_23      -0.0128027000
_diffrn_orient_matrix_UB_31      0.0827665000
_diffrn_orient_matrix_UB_32      -0.0156570000
_diffrn_orient_matrix_UB_33      0.0439255000
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_av_unetI/netI     0.1021
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28972
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.247
_diffrn_reflns_theta_min         3.144
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    4.666
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       needle
_exptl_crystal_F_000             3244
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     844
_refine_ls_number_reflns         12492
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0520P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1337
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8206
_reflns_number_total             12492
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc03431e2.cif
_cod_data_source_block           xdpm75
_cod_database_code               1552336
_manchester_internal_coll_name   xdpm75
_manchester_internal_coll_client HN/SWL/CAPG
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 7/12s
_manchester_internal_coll_frame_width 1.0
_manchester_internal_coll_frame_method '\w & \f scans'
_manchester_internal_coll_user   CAPG/HN
_manchester_internal_coll_date   02/8/17
_manchester_internal_process_user CAPG
_manchester_internal_process_date 02/8/17
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 03/8/17
_manchester_internal_refinement_user CAPG
_manchester_internal_refinement_date 24/8/17
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         Yb(N(SiC9H21)2)2B(C6F5)4CH2Cl2
_shelx_estimated_absorpt_t_max   0.653
_shelx_estimated_absorpt_t_min   0.335
_reflns_odcompleteness_completeness 98.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 Cl2-C61 = Cl1-C61
 1.753 with sigma of 0.02
3. Rigid bond restraints
 C61, Cl1, Cl2, H61A, H61B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C61 \\sim Cl1 \\sim Cl2 \\sim H61A \\sim H61B: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.01
5.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)
5.b Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B)
5.c 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              66860
_olex2_date_sample_completion    2017-08-03
_olex2_date_sample_data_collection 2017-08-02
_olex2_date_sample_submission    2017-08-02
_olex2_exptl_crystal_mounting_method 'From fomblin on a microscope slide.'
_olex2_submission_original_sample_id XDPM75
_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 1.840
_oxdiff_exptl_absorpt_empirical_full_min 0.641