Reactivity of Bulky Formamidinatosamarium(II or III) Complexes with C═O and C═S Bonds.
Deacon, Glen B.; Junk, Peter C.; Wang, Jun; Werner, Daniel; Inorganic chemistry  (2014) 141110081832000–; doi:10.1021/ic502181g

data_4341599
_publ_section_title
;
 Reactivity of Bulky Formamidinatosamarium(II or III) Complexes with
 C&#x2550;O and C&#x2550;S Bonds.
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              141110081832000
_journal_paper_doi               10.1021/ic502181g
_journal_year                    2014
_chemical_formula_moiety         '2(C55 H78 N4 O S2 Sm), 6(C6 H6)'
_chemical_formula_sum            'C146 H156 D36 N8 O2 S4 Sm2'
_chemical_formula_weight         2556.23
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-08-30
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.8760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.8749(3)
_cell_length_b                   23.1663(6)
_cell_length_c                   19.3292(3)
_cell_measurement_temperature    123(1)
_cell_volume                     6765.4(2)
_computing_cell_refinement       'Bruker Apex2 v2.0 (Bruker AXS, 2005)'
_computing_data_collection       'Bruker Apex2 v2.0 (Bruker AXS, 2005)'
_computing_data_reduction        'Bruker Apex2 v2.0 (Bruker AXS, 2005)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker X8 Apex II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            55162
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.609
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.974
_exptl_absorpt_correction_T_max  0.9261
_exptl_absorpt_correction_T_min  0.7268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.850
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         15524
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0787
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12834
_reflns_number_total             15524
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502181g_si_001.cif
_cod_data_source_block           Compound5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 
;
_cod_database_code               4341599
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.727
_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
 C57-C58 = C58-C59 = C59-C60 = C60-C61 = C61-C62 = C62-C57
 1.39 with sigma of 0.02
 C80-C81 = C81-C82 = C82-C83 = C83-C84 = C84-C85 = C85-C80
 1.39 with sigma of 0.02
 C69-C70 = C70-C71 = C71-C72 = C72-C73 = C73-C74 = C74-C69
 1.39 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C57) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq: with sigma of
0.002 and sigma for terminal atoms of 0.004
4. Others
 Fixed Sof: S1(0.5) C1(0.5) S2(0.5) C2(0.5) S3(0.5) S4(0.5) C57(0.5) H57(0.5)
 C58(0.5) H58(0.5) C59(0.5) H59(0.5) C60(0.5) H60(0.5) C61(0.5) H61(0.5)
 C62(0.5) H62(0.5) C81(0.5) H81(0.5) C82(0.5) H82(0.5) C83(0.5) H83(0.5)
 C80(0.5) H80(0.5) C84(0.5) H84(0.5) C85(0.5) H85(0.5)
5.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C22(H22), C25(H25), C34(H34), C37(H37), C47(H47), C50(H50)
5.b Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B)
5.c Me refined with riding coordinates:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C),
 C39(H39A,H39B,H39C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,
 H51C), C52(H52A,H52B,H52C)
5.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C15(H15), C18(H18), C19(H19), C20(H20), C30(H30),
 C31(H31), C32(H32), C40(H40), C43(H43), C44(H44), C45(H45), C57(H57), C58(H58),
  C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65),
 C66(H66), C67(H67), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72), C73(H73),
  C74(H74), C81(H81), C82(H82), C83(H83), C80(H80), C84(H84), C85(H85)
;
_olex2_submission_special_instructions 'No special instructions were received'