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_7704027
_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         'C40 H56 N4 O2 Sm2, C7 H8'
_chemical_formula_sum            'C47 H64 N4 O2 Sm2'
_chemical_formula_weight         1017.72
_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     direct
_audit_creation_date             2019-05-20
_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                 108.706(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.9470(8)
_cell_length_b                   21.5868(6)
_cell_length_c                   23.2649(9)
_cell_measurement_reflns_used    8186
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.0950
_cell_measurement_theta_min      3.2950
_cell_volume                     8537.1(6)
_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    'ShelXS (Sheldrick, 2008)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.991
_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    -64.00  30.00   1.00    3.00    --  -37.19  77.00  30.00   94
  2  \w   -108.00 -44.00   1.00    3.00    --  -37.19-167.00  46.00   64
  3  \w    -54.00  30.00   1.00    3.00    --  -37.19  57.00  90.00   84
  4  \w    -32.00  56.00   1.00    3.00    --   37.19 -38.00-180.00   88
  5  \w     20.00 104.00   1.00    3.00    --   37.19  57.00  30.00   84
  6  \w      8.00 109.00   1.00    3.00    --   37.19  19.00   0.00  101
  7  \w     23.00  91.00   1.00    3.00    --   37.19-125.00 150.00   68
  8  \w    -30.00  64.00   1.00    3.00    --   37.19 -77.00-180.00   94
  9  \w     41.00 132.00   1.00   10.00    --  111.00 -30.00  90.00   91
 10  \w    100.00 178.00   1.00   10.00    --  111.00 111.00-150.00   78
 11  \w     41.00 116.00   1.00   10.00    --  111.00-111.00  90.00   75
 12  \w     43.00 128.00   1.00   10.00    --  111.00 -45.00-150.00   85
 13  \w     93.00 178.00   1.00   10.00    --  111.00  61.00  90.00   85
 14  \w     90.00 178.00   1.00   10.00    --  111.00  30.00-150.00   88
 15  \w     42.00 109.00   1.00   10.00    --  111.00 -94.00 -30.00   67
 16  \w     44.00 129.00   1.00   10.00    --  111.00 -61.00  90.00   85
 17  \w     42.00 109.00   1.00   10.00    --  111.00 -94.00 -60.00   67
 18  \w     84.00 178.00   1.00   10.00    --  111.00  77.00 150.00   94
 19  \w    -86.00   6.00   1.00    3.00    --  -37.19 116.00 -78.00   92
 20  \w   -105.00 -10.00   1.00    3.00    --  -37.19 -77.00-150.00   95
 21  \w    -30.00  54.00   1.00    3.00    --   37.19 -57.00 -90.00   84
 22  \w     20.00 104.00   1.00    3.00    --   37.19  57.00-120.00   84
 23  \w     10.00 105.00   1.00    3.00    --   37.19  77.00 150.00   95
 24  \w     10.00 105.00   1.00    3.00    --   37.19  77.00  60.00   95
 25  \w     20.00 104.00   1.00    3.00    --   37.19  57.00 150.00   84
 26  \w     18.00 106.00   1.00    3.00    --   37.19  38.00   0.00   88
 27  \w     10.00 105.00   1.00    3.00    --   37.19  77.00 -60.00   95
 28  \w     90.00 156.00   1.00   10.00    --  111.00  30.00 -60.00   66
;
_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      0.0630172000
_diffrn_orient_matrix_UB_12      -0.0456294000
_diffrn_orient_matrix_UB_13      0.0373179000
_diffrn_orient_matrix_UB_21      0.0071765000
_diffrn_orient_matrix_UB_22      0.0372261000
_diffrn_orient_matrix_UB_23      0.0580728000
_diffrn_orient_matrix_UB_31      -0.0646648000
_diffrn_orient_matrix_UB_32      -0.0402777000
_diffrn_orient_matrix_UB_33      0.0113529000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            9870
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.402
_diffrn_reflns_theta_min         3.309
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.763
_exptl_absorpt_correction_T_max  0.412
_exptl_absorpt_correction_T_min  0.135
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_description       block
_exptl_crystal_F_000             4112
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.580
_refine_diff_density_min         -2.335
_refine_diff_density_rms         0.174
_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     546
_refine_ls_number_reflns         9870
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0659
_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^)+(0.1220P)^2^+39.6362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1888
_refine_ls_wR_factor_ref         0.2030
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7265
_reflns_number_total             9870
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9816\% 
 around [0.92 0.00 -0.38] (reciprocal) or [1.00 -0.00 0.00] (direct)
;
_cod_data_source_file            d0dt01095b2.cif
_cod_data_source_block           L2Sm4(mu-O)2(thf)2
_cod_depositor_comments
'Adding full bibliography for 7704024--7704027.cif.'
_cod_database_code               7704027
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C50H61N4O2Sm2
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5896(19)
 0.4104(19)
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. Restrained distances
 O3-C39 \\sim O3-C39A
 with sigma of 0.02
 C39-C40 \\sim C39A-C40A
 with sigma of 0.02
 O3-C40 \\sim O3-C40A
 with sigma of 0.04
 O2-C37 \\sim O2-C37A
 with sigma of 0.02
 C38-C37 \\sim C38A-C37A
 with sigma of 0.02
 O2-C38 \\sim O2-C38A
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
O3 \\sim C39 \\sim C39A \\sim C40 \\sim C40A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
O2 \\sim C37 \\sim C37A \\sim C38 \\sim C38A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
5. Others
 Sof(C39A)=Sof(H39C)=Sof(H39D)=Sof(C40A)=Sof(H40C)=Sof(H40D)=1-FVAR(1)
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=FVAR(1)
 Sof(C37A)=Sof(H37C)=Sof(H37D)=Sof(C38A)=Sof(H38C)=Sof(H38D)=1-FVAR(2)
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=Sof(H38B)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C5(H5), C6(H6), C10(H10), C23(H23), C24(H24), C28(H28)
6.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B), C29(H29A,
 H29B), C31(H31A,H31B), C33(H33A,H33B), C35(H35A,H35B), C37(H37A,H37B),
 C37A(H37C,H37D), C38(H38A,H38B), C38A(H38C,H38D), C39(H39A,H39B), C39A(H39C,
 H39D), C40(H40A,H40B), C40A(H40C,H40D)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C19(H19), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
6.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C36(H36A,
 H36B,H36C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              13396
_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 3.011
_oxdiff_exptl_absorpt_empirical_full_min 0.613
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2