Alkali-metal- and halide-free dinuclear mixed-valent samarium and europium complexes.
Mukthar, Nishya F. M.; Schley, Nathan D.; Ung, Gaël; Dalton transactions (Cambridge, England : 2003) 49 (2020) 16059–16061; doi:10.1039/d0dt01095b

data_7704024
_publ_section_title
;
 Alkali-metal- and halide-free dinuclear mixed-valent samarium and
 europium complexes.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16059
_journal_page_last               16061
_journal_paper_doi               10.1039/d0dt01095b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C48 H84 N6 Si4 Sm2'
_chemical_formula_sum            'C48 H84 N6 Si4 Sm2'
_chemical_formula_weight         1158.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-17 deposited with the CCDC.	2020-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                79.168(2)
_cell_angle_beta                 79.681(2)
_cell_angle_gamma                76.855(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4659(3)
_cell_length_b                   11.7021(3)
_cell_length_c                   21.3015(6)
_cell_measurement_reflns_used    31714
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.0520
_cell_measurement_theta_min      2.8870
_cell_volume                     2705.71(13)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1506
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.904
_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    -20.00  57.00   1.00    5.00    --   18.41 -99.00-120.00   77
  2  \w     -8.00  86.00   1.00    5.00    --   18.41  77.00   0.00   94
  3  \w    -53.00  48.00   1.00    5.00    --   18.41 -19.00-150.00  101
  4  \w     -8.00  86.00   1.00    5.00    --   18.41  77.00 120.00   94
  5  \w    -49.00  35.00   1.00    5.00    --   18.41 -57.00 -90.00   84
  6  \w    -49.00  35.00   1.00    5.00    --   18.41 -57.00-180.00   84
  7  \w    -88.00   0.00   1.00    5.00    --  -18.49 -38.00 -60.00   88
  8  \w    -51.00  37.00   1.00    5.00    --   18.41 -38.00  60.00   88
  9  \w      2.00  86.00   1.00    5.00    --   18.41  57.00-120.00   84
 10  \w    -20.00  57.00   1.00    5.00    --   18.41 -99.00 -30.00   77
 11  \w    -20.00  57.00   1.00    5.00    --   18.41 -99.00 120.00   77
 12  \w    -51.00  37.00   1.00    5.00    --   18.41 -38.00   0.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0241677000
_diffrn_orient_matrix_UB_12      0.0162285000
_diffrn_orient_matrix_UB_13      0.0246885000
_diffrn_orient_matrix_UB_21      0.0357625000
_diffrn_orient_matrix_UB_22      -0.0580281000
_diffrn_orient_matrix_UB_23      0.0052916000
_diffrn_orient_matrix_UB_31      0.0475003000
_diffrn_orient_matrix_UB_32      0.0183661000
_diffrn_orient_matrix_UB_33      -0.0231451000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            65776
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.276
_diffrn_reflns_theta_min         2.288
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.274
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.183
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       block
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.399
_exptl_crystal_size_mid          0.386
_exptl_crystal_size_min          0.275
_refine_diff_density_max         2.705
_refine_diff_density_min         -1.252
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         14653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0192P)^2^+8.5419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0850
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13019
_reflns_number_total             14653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01095b2.cif
_cod_data_source_block           LSm2(HMDS)2
_cod_depositor_comments
'Adding full bibliography for 7704024--7704027.cif.'
_cod_database_code               7704024
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C48H84N6Si4Sm2
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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.a Ternary CH refined with riding coordinates:
 C14(H14), C15(H15), C23(H23), C32(H32), C41(H41), C42(H42)
2.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C20(H20A,H20B), C27(H27A,H27B), C29(H29A,H29B), C36(H36A,
 H36B), C38(H38A,H38B), C45(H45A,H45B), C47(H47A,H47B)
2.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C33(H33)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C19(H19A,H19B,
 H19C), C21(H21A,H21B,H21C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C37(H37A,
 H37B,H37C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              44459
_olex2_date_sample_data_collection 2018-12-12
_olex2_exptl_crystal_mounting_method 'mounted in a polyimide loop'
_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 1.573
_oxdiff_exptl_absorpt_empirical_full_min 0.594