Bis(amidinate) ligands in early lanthanide chemistry - synthesis, structures, and hydroamination catalysis.
Kazeminejad, Neda; Munzel, Denise; Gamer, Michael T.; Roesky, Peter W.; Chemical communications (Cambridge, England) 53 (2017) 1060–1063; doi:10.1039/c6cc08958e

data_7119283
_publ_section_title
;
 Bis(amidinate) ligands in early lanthanide chemistry - synthesis,
 structures, and hydroamination catalysis.
;
_journal_issue                   6
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1060
_journal_page_last               1063
_journal_paper_doi               10.1039/c6cc08958e
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C104 H120 N10 O4 Si4 Sm2, 3(C4 H8 O)'
_chemical_formula_sum            'C116 H144 N10 O7 Si4 Sm2'
_chemical_formula_weight         2203.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-11-09 deposited with the CCDC.
2016-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                82.107(9)
_cell_angle_beta                 81.378(9)
_cell_angle_gamma                68.045(8)
_cell_formula_units_Z            2
_cell_length_a                   16.7981(17)
_cell_length_b                   18.7804(19)
_cell_length_c                   19.323(2)
_cell_measurement_reflns_used    19780
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      1.31
_cell_volume                     5567.9(10)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2009)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED & LANA, PLATON (A.L.Spek, 2009)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'image plate (34cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE image plate'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       'two-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.5mm monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.1240
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37109
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.132
_diffrn_reflns_theta_min         1.315
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    1.145
_exptl_absorpt_correction_T_max  0.8470
_exptl_absorpt_correction_T_min  0.6418
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       prism
_exptl_crystal_F_000             2292
_exptl_crystal_size_max          0.535
_exptl_crystal_size_mid          0.359
_exptl_crystal_size_min          0.159
_refine_diff_density_max         1.801
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.841
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1169
_refine_ls_number_reflns         21650
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      0.839
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0766P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1429
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11795
_reflns_number_total             21650
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc08958e2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7119278--7119283.cif.'
_cod_original_cell_volume        5567.9(11)
_cod_database_code               7119283
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 Si4A-C96A
 1.9 with sigma of 0.002
 Si4B-C96B
 1.9 with sigma of 0.002
 C115-C116
 1.53 with sigma of 0.002
 C111-C112
 1.53 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
C27A \\sim C27B: within 1.7A with sigma of 0.004 and sigma for terminal atoms
of 0.008
O4 \\sim C1C \\sim C1D \\sim C104 \\sim C105: within 1.7A with sigma of 0.008
and sigma for terminal atoms of 0.016
C1A \\sim C1B \\sim C102 \\sim C103: within 1.7A with sigma of 0.008 and sigma
for terminal atoms of 0.016
Uanis(C96A) = Uanis(C97A)
Uanis(C97B) = Uanis(C96B)
4. Rigid body (RIGU) restrains
 C22A, C23A, C24A, C25A, C26A, C27A, C28A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C22B, C23B, C24B, C25B, C26B, C27B, C28B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Si4A(0.4) Si4B(0.6) H95d(0.6) H95e(0.6) H95f(0.6) H95a(0.4)
 H95b(0.4) H95c(0.4) C1A(0.7) H1Aa(0.7) H1Ab(0.7) C1B(0.7) H1Ba(0.7) H1Bb(0.7)
 C22A(0.7) C23A(0.7) H23A(0.7) C24A(0.7) H24A(0.7) C25A(0.7) C26A(0.7)
 H26A(0.7) C27A(0.7) H27A(0.7) C28A(0.7) H28a(0.7) H28b(0.7) H28c(0.7)
 C96A(0.4) H96a(0.4) H96b(0.4) H96c(0.4) C97A(0.4) H97a(0.4) H97b(0.4)
 H97c(0.4) C102(0.7) H10e(0.7) H10f(0.7) C103(0.7) H10g(0.7) H10h(0.7) C1C(0.3)
 H1Ca(0.3) H1Cb(0.3) C1D(0.3) H1Da(0.3) H1Db(0.3) C25B(0.3) C26B(0.3) H26B(0.3)
 C27B(0.3) H27B(0.3) C22B(0.3) C23B(0.3) H23B(0.3) C24B(0.3) H24B(0.3)
 C28B(0.3) H28d(0.3) H28e(0.3) H28f(0.3) C96B(0.6) H96d(0.6) H96e(0.6)
 H96f(0.6) C97B(0.6) H97d(0.6) H97e(0.6) H97f(0.6) C104(0.3) H10i(0.3)
 H10j(0.3) C105(0.3) H10k(0.3) H10l(0.3)
6.a Secondary CH2 refined with riding coordinates:
 C98(H98a,H98b), C99(H99a,H99b), C100(H10a,H10b), C101(H10c,H10d), C1A(H1Aa,
 H1Ab), C1B(H1Ba,H1Bb), C102(H10e,H10f), C103(H10g,H10h), C1C(H1Ca,H1Cb),
 C1D(H1Da,H1Db), C104(H10i,H10j), C105(H10k,H10l), C110(H11a,H11b), C111(H11c,
 H11d), C112(H11e,H11f), C113(H11g,H11h), C106(H10m,H10n), C107(H10o,H10p),
 C108(H10q,H10r), C109(H10s,H10t), C114(H11i,H11j), C115(H11k,H11l), C116(H11m,
 H11n), C117(H11o,H11p)
6.b Me refined with riding coordinates:
 C95(H95d,H95e,H95f), C95(H95a,H95b,H95c)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C20(H20), C16(H16),
 C17(H17), C19(H19), C34(H34), C33(H33), C31(H31), C30(H30), C37(H37), C38(H38),
  C40(H40), C41(H41), C47(H47), C46(H46), C45(H45), C54(H54), C53(H53),
 C55(H55), C62(H62), C60(H60), C59(H59), C63(H63), C69(H69), C67(H67), C66(H66),
  C70(H70), C73(H73), C77(H77), C76(H76), C74(H74), C84(H84), C83(H83),
 C81(H81), C80(H80), C23A(H23A), C24A(H24A), C26A(H26A), C27A(H27A), C26B(H26B),
  C27B(H27B), C23B(H23B), C24B(H24B)
6.d Fitted hexagon refined as free rotating group:
 C6(C7,C2,C3,C4,C5), C13(C8,C9,C10,C11,C12), C20(C15,C16,C17,C18,C19), C29(C34,
 C33,C32,C31,C30), C37(C38,C39,C40,C41,C36), C48(C47,C46,C45,C44,C49), C54(C53,
 C52,C51,C56,C55), C62(C61,C60,C59,C58,C63), C69(C68,C67,C66,C65,C70), C73(C72,
 C77,C76,C75,C74), C79(C84,C83,C82,C81,C80), C25B(C26B,C27B,C22B,C23B,C24B)
6.e Idealised Me refined as rotating group:
 C21(H21a,H21b,H21c), C35(H35a,H35b,H35c), C42(H42a,H42b,H42c), C64(H64a,H64b,
 H64c), C71(H71a,H71b,H71c), C78(H78a,H78b,H78c), C85(H85a,H85b,H85c), C86(H86a,
 H86b,H86c), C87(H87a,H87b,H87c), C88(H88a,H88b,H88c), C89(H89a,H89b,H89c),
 C90(H90a,H90b,H90c), C91(H91a,H91b,H91c), C92(H92a,H92b,H92c), C93(H93a,H93b,
 H93c), C94(H94a,H94b,H94c), C28A(H28a,H28b,H28c), C96A(H96a,H96b,H96c),
 C97A(H97a,H97b,H97c), C28B(H28d,H28e,H28f), C96B(H96d,H96e,H96f), C97B(H97d,
 H97e,H97f)
;
_shelx_res_checksum              55055
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'