Heteroleptic samarium(iii) halide complexes probed by fluorescence-detected L<sub>3</sub>-edge X-ray absorption spectroscopy.
Goodwin, Conrad A. P.; Réant, Benjamin L L; Kragskow, Jon G. C.; DiMucci, Ida M.; Lancaster, Kyle M.; Mills, David P.; Sproules, Stephen; Dalton transactions (Cambridge, England : 2003) 47 (2018) 10613–10625; doi:10.1039/c8dt01452c

data_7046251
_publ_section_title
;
 Heteroleptic samarium(iii) halide complexes probed by
 fluorescence-detected L<sub>3</sub>-edge X-ray absorption spectroscopy.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10613
_journal_page_last               10625
_journal_paper_doi               10.1039/c8dt01452c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C36 H84 I N2 Si4 Sm, 0.5(C6 H14)'
_chemical_formula_sum            'C39 H91 I N2 Si4 Sm'
_chemical_formula_weight         977.74
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-04-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2018-04-28 deposited with the CCDC.
2018-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.0340(4)
_cell_length_b                   20.2409(4)
_cell_length_c                   24.0385(5)
_cell_measurement_reflns_used    11905
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      28.6260
_cell_measurement_theta_min      2.6340
_cell_volume                     9747.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -34.00  39.80   0.90    2.00    --  -17.77  57.00 120.00   82
  2  \w    -80.00 -53.00   0.90    2.00    --  -17.77 137.00  16.00   30
  3  \w      1.00  40.60   0.90    2.00    --   18.86 -37.00-180.00   44
  4  \w    -86.00  11.20   0.90    2.00    --  -17.77 -77.00-180.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0082720000
_diffrn_orient_matrix_UB_12      -0.0337615000
_diffrn_orient_matrix_UB_13      -0.0037865000
_diffrn_orient_matrix_UB_21      0.0309992000
_diffrn_orient_matrix_UB_22      0.0093072000
_diffrn_orient_matrix_UB_23      -0.0119125000
_diffrn_orient_matrix_UB_31      0.0150047000
_diffrn_orient_matrix_UB_32      -0.0005845000
_diffrn_orient_matrix_UB_33      0.0267312000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            39822
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.217
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.963
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       block
_exptl_crystal_F_000             4080
_exptl_crystal_preparation       'By Jon Kragskow and CAPG.'
_exptl_crystal_recrystallization_method 'From hexane.'
_exptl_crystal_size_max          0.381
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.172
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.103
_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         8929
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0194P)^2^+11.4398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7087
_reflns_number_total             8929
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01452c2.cif
_cod_data_source_block           2-I
_cod_depositor_comments
'Adding full bibliography for 7046250--7046253.cif.'
_cod_database_code               7046251
_manchester_internal_coll_name   adpm350
_manchester_internal_coll_client CAPG
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 2.0
_manchester_internal_coll_frame_width 0.9
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   CAPG
_manchester_internal_coll_date   13/7/16
_manchester_internal_process_user CAPG
_manchester_internal_process_date 27/3/18
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 27/3/18
_manchester_internal_refinement_user CAPG
_manchester_internal_refinement_date 28/4/18
_manchester_internal_validation_user CAPG
_manchester_internal_validation_date 28/4/18
_manchester_internal_archive_date 28/4/18
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         Sm(N(SiC9H21)2)2I
_shelx_estimated_absorpt_t_max   0.757
_shelx_estimated_absorpt_t_min   0.522
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 C38-C37 = C38-C39 = C39-C40 = C40-C41 = C42-C41
 1.51 with sigma of 0.01
 C37-C39
 2.45 with sigma of 0.01
 C38-C40
 2.45 with sigma of 0.01
 C39-C41
 2.45 with sigma of 0.01
 C40-C42
 2.45 with sigma of 0.01
3. Others
 Fixed Sof: C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5) C38(0.5) H38A(0.5)
 H38B(0.5) C39(0.5) H39A(0.5) H39B(0.5) C40(0.5) H40A(0.5) H40B(0.5) C41(0.5)
 H41A(0.5) H41B(0.5) C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5)
4.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)
4.b Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B)
4.c Me refined with riding coordinates:
 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), C37(H37A,H37B,H37C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              30048
_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 1.343
_oxdiff_exptl_absorpt_empirical_full_min 0.814