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_1552335
_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 Cl N2 Si4 Tm'
_chemical_formula_sum            'C36 H84 Cl N2 Si4 Tm'
_chemical_formula_weight         861.79
_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
_audit_creation_date             2017-07-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-11-23 deposited with the CCDC.    2019-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.043(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8309(4)
_cell_length_b                   13.1077(3)
_cell_length_c                   22.5379(6)
_cell_measurement_reflns_used    17724
_cell_measurement_temperature    100.00(2)
_cell_measurement_theta_max      29.8500
_cell_measurement_theta_min      3.5910
_cell_volume                     4420.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(2)
_diffrn_detector                 'CCD plate'
_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    -45.00 -19.00   0.50    4.00    --    5.00 -43.00  -7.00   52
  2  \w     36.00  62.00   0.50    4.00    --   -7.50  43.00 143.00   52
  3  \w     48.00  81.00   0.50    4.00    --   -7.50  57.00-150.00   66
  4  \w    -34.00  81.00   0.50    4.00    --   -7.50  57.00  60.00  230
  5  \w    -39.00  36.00   0.50    4.00    --   -7.50  57.00-150.00  150
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0420198000
_diffrn_orient_matrix_UB_12      -0.0109465000
_diffrn_orient_matrix_UB_13      0.0034730000
_diffrn_orient_matrix_UB_21      0.0217998000
_diffrn_orient_matrix_UB_22      -0.0269694000
_diffrn_orient_matrix_UB_23      0.0281282000
_diffrn_orient_matrix_UB_31      0.0027733000
_diffrn_orient_matrix_UB_32      0.0456349000
_diffrn_orient_matrix_UB_33      0.0174376000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31900
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.346
_diffrn_reflns_theta_min         3.528
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.201
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.382
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.435
_exptl_crystal_size_mid          0.301
_exptl_crystal_size_min          0.217
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         8039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0185
_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^)+(0.0259P)^2^+2.0752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0468
_refine_ls_wR_factor_ref         0.0476
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7461
_reflns_number_total             8039
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc03431e2.cif
_cod_data_source_block           rdpm43
_cod_database_code               1552335
_manchester_internal_coll_name   rdpm43
_manchester_internal_coll_client CAPG/HN/SWL
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 4s
_manchester_internal_coll_frame_width 0.5
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   CAPG
_manchester_internal_coll_date   22/07/17
_manchester_internal_process_user CAPG
_manchester_internal_process_date 22/07/17
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 22/07/17
_manchester_internal_refinement_user CAPG
_manchester_internal_refinement_date 23/07/17
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         Tm(N(SiC9H21)2)2Cl
_diffrn_oxdiff_ac3_digest_frames
;
01b77e4d215d63a35a73e869239285d3ca005508110
;
_diffrn_oxdiff_ac3_digest_hkl
;
0126995b4cf046dd8f7519cd58329d36bb86a8
;
_reflns_odcompleteness_completeness 98.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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              81991
_olex2_date_sample_data_collection 2017-07-22
_olex2_date_sample_submission    2017-07-22
_olex2_exptl_crystal_mounting_method 'From fomblin 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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.720
_oxdiff_exptl_absorpt_empirical_full_min 0.493