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_7704025
_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 Eu2 N6 Si4'
_chemical_formula_sum            'C48 H84 Eu2 N6 Si4'
_chemical_formula_weight         1161.49
_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             2019-05-21
_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                79.337(4)
_cell_angle_beta                 79.682(4)
_cell_angle_gamma                77.099(4)
_cell_formula_units_Z            2
_cell_length_a                   11.4426(5)
_cell_length_b                   11.6392(5)
_cell_length_c                   21.2371(9)
_cell_measurement_reflns_used    9282
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      27.7820
_cell_measurement_theta_min      2.8620
_cell_volume                     2681.2(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      100.01(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 0.884
_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    -51.00  37.00   1.00   32.50    --   18.25 -38.00  60.00   88
  2  \w     -8.00  86.00   1.00   32.50    --   18.25  77.00 -60.00   94
  3  \w     -8.00  86.00   1.00   32.50    --   18.25  77.00  60.00   94
  4  \w     -8.00  86.00   1.00   32.50    --   18.25  77.00-180.00   94
  5  \w    -49.00  35.00   1.00   32.50    --   18.25 -57.00-150.00   84
  6  \w    -11.00  90.00   1.00   32.50    --   18.25  19.00-120.00  101
  7  \w    -49.00  35.00   1.00   32.50    --   18.25 -57.00 150.00   84
  8  \w    -49.00 -24.00   1.00   32.50    --   18.25 -77.00 -60.00   25
  9  \w    -45.00  45.00   1.00   32.50    --  -18.49  77.00  30.00   90
;
_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      -0.0284960000
_diffrn_orient_matrix_UB_12      0.0066567000
_diffrn_orient_matrix_UB_13      -0.0278544000
_diffrn_orient_matrix_UB_21      0.0475818000
_diffrn_orient_matrix_UB_22      -0.0436793000
_diffrn_orient_matrix_UB_23      -0.0127817000
_diffrn_orient_matrix_UB_31      -0.0324576000
_diffrn_orient_matrix_UB_32      -0.0452534000
_diffrn_orient_matrix_UB_33      0.0154988000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1208
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            14131
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.295
_diffrn_reflns_theta_min         2.471
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.444
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.639
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       needle
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.038
_refine_diff_density_max         2.878
_refine_diff_density_min         -2.005
_refine_diff_density_rms         0.213
_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     562
_refine_ls_number_reflns         14131
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0382P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1237
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9540
_reflns_number_total             14131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01095b2.cif
_cod_data_source_block           LEu2(HMDS)2
_cod_depositor_comments
'Adding full bibliography for 7704024--7704027.cif.'
_cod_database_code               7704025
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C48H84Eu2N6Si4
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8601(18)
 0.1399(18)
2. 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
3.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), C12(H12), C17(H17)
3.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C23(H23A,H23B), C25(H25A,H25B), C27(H27A,H27B), C29(H29A,
 H29B), C31(H31A,H31B), C33(H33A,H33B), C35(H35A,H35B)
3.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C18(H18)
3.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C28(H28A,H28B,
 H28C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C36(H36A,
 H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,
 H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              78159
_olex2_date_sample_data_collection 2019-05-20
_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 1.524
_oxdiff_exptl_absorpt_empirical_full_min 0.591