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_1552334
_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         'C24 B F20, C36 H84 N2 Si4 Sm'
_chemical_formula_sum            'C60 H84 B F20 N2 Si4 Sm'
_chemical_formula_weight         1486.81
_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             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                90
_cell_angle_beta                 114.818(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.9284(3)
_cell_length_b                   17.0513(2)
_cell_length_c                   21.1049(4)
_cell_measurement_reflns_used    41785
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      73.4170
_cell_measurement_theta_min      2.5410
_cell_volume                     6509.2(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  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     70.71 257.71   1.00   10.00    --  100.00  73.87 -25.79  187
  2  \w     77.92 261.92   1.00   10.00    --  105.00  73.87 129.21  184
  3  \f     54.43 325.77   1.00   10.00  14.82 -70.00  73.87    --   271
  4  \f    -23.96 326.48   1.00   10.00 158.57 105.00  73.87    --   350
  5  \f    -19.93 277.26   1.00   10.00  74.83  55.00  73.87    --   297
  6  \w     32.88 103.88   1.00   10.00    --  -35.00  73.87  89.21   71
  7  \f    -25.10 265.26   1.00   10.00 167.64  80.00  73.87    --   290
  8  \w    -71.60  62.40   1.00   10.00    --  -75.00  73.87-165.79  134
  9  \f    -25.79 181.34   1.00   10.00 136.84  95.00  73.87    --   207
 10  \w     58.71 197.71   1.00   10.00    --   40.00  73.87 169.21  139
 11  \f     85.32 325.47   1.00   10.00  85.84 110.00  73.87    --   240
 12  \w    123.21 268.21   1.00   10.00    --  111.00  73.87  74.21  145
 13  \w    122.34 256.34   1.00   10.00    --  110.00  73.87 -40.79  134
 14  \w     92.08 209.08   1.00   10.00    --   80.00  73.87  29.21  117
 15  \w    -27.47 116.53   1.00   10.00    --   -2.00  73.87 149.21  144
 16  \f    136.94 333.06   1.00   10.00 144.21 110.00  73.87    --   196
;
_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      0.0077671000
_diffrn_orient_matrix_UB_12      0.0595386000
_diffrn_orient_matrix_UB_13      -0.0514425000
_diffrn_orient_matrix_UB_21      -0.0668276000
_diffrn_orient_matrix_UB_22      0.0458092000
_diffrn_orient_matrix_UB_23      -0.0007480000
_diffrn_orient_matrix_UB_31      0.0522606000
_diffrn_orient_matrix_UB_32      0.0501507000
_diffrn_orient_matrix_UB_33      0.0618695000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0790
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            71543
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         2.561
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.338
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01770
_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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       block
_exptl_crystal_F_000             3044
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.641
_refine_diff_density_min         -1.339
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     817
_refine_ls_number_reflns         11897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+2.8187P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10921
_reflns_number_total             11897
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc03431e2.cif
_cod_data_source_block           xdpm66
_cod_database_code               1552334
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         Sm(N(SiC9H21)2)2B(C6F5)4
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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              99587
_manchester_internal_coll_client CAPG
_manchester_internal_coll_date   15/2/17
_manchester_internal_coll_frame_method '\w and \f scans'
_manchester_internal_coll_frame_time 10.0
_manchester_internal_coll_frame_width 1.0
_manchester_internal_coll_name   xdpm66
_manchester_internal_coll_type   custom
_manchester_internal_coll_user   CAPG
_manchester_internal_process_date 16/2/17
_manchester_internal_process_user CAPG
_manchester_internal_refinement_date 16/2/17
_manchester_internal_refinement_user CAPG
_manchester_internal_solution_date 16/2/17
_manchester_internal_solution_user CAPG
_olex2_exptl_crystal_mounting_method 'From fombin on a microscope slide.'
_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 36.154
_oxdiff_exptl_absorpt_empirical_full_min 0.306