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_7704026
_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         'C46 H74 Eu2 N5 O Si2'
_chemical_formula_sum            'C46 H74 Eu2 N5 O Si2'
_chemical_formula_weight         1073.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-02
_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                90
_cell_angle_beta                 90.855(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7438(4)
_cell_length_b                   20.1221(6)
_cell_length_c                   17.6945(4)
_cell_measurement_reflns_used    14378
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.9050
_cell_measurement_theta_min      2.9490
_cell_volume                     4892.9(2)
_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      100.00(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 0.906
_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    -49.00  35.00   1.00   15.00    --   18.41 -57.00  60.00   84
  2  \w    -20.00  57.00   1.00   15.00    --   18.41 -99.00 -60.00   77
  3  \w     35.00  91.00   1.00   15.00    --   18.41 178.00  90.00   56
  4  \w      0.00  88.00   1.00   15.00    --   18.41  38.00-120.00   88
  5  \w    -11.00  90.00   1.00   15.00    --   18.41  19.00  30.00  101
  6  \w     34.00  89.00   1.00   15.00    --   18.41-178.00 -90.00   55
  7  \w      2.00  86.00   1.00   15.00    --   18.41  57.00  90.00   84
;
_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      -0.0283794000
_diffrn_orient_matrix_UB_12      0.0161223000
_diffrn_orient_matrix_UB_13      0.0276748000
_diffrn_orient_matrix_UB_21      -0.0382113000
_diffrn_orient_matrix_UB_22      0.0042064000
_diffrn_orient_matrix_UB_23      -0.0269478000
_diffrn_orient_matrix_UB_31      -0.0199268000
_diffrn_orient_matrix_UB_32      -0.0310639000
_diffrn_orient_matrix_UB_33      0.0107620000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30304
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.240
_diffrn_reflns_theta_min         2.329
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.626
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.292
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       plate
_exptl_crystal_F_000             2188
_exptl_crystal_size_max          0.306
_exptl_crystal_size_mid          0.249
_exptl_crystal_size_min          0.045
_refine_diff_density_max         3.196
_refine_diff_density_min         -1.203
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         6620
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0400P)^2^+23.5640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0998
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5542
_reflns_number_total             6620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01095b2.cif
_cod_data_source_block           LEu2(HMDS)(thf)
_cod_depositor_comments
'Adding full bibliography for 7704024--7704027.cif.'
_cod_database_code               7704026
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C46H74Eu2N5OSi2
_reflns_odcompleteness_completeness 99.90
_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:
 C2(H2), C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C8(H8A,H8B), C15(H15A,H15B), C17(H17A,H17B), C19(H19A,H19B),
 C20(H20A,H20B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C12(H12)
2.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              97988
_olex2_date_sample_data_collection 2019-03-01
_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 2.018
_oxdiff_exptl_absorpt_empirical_full_min 0.522