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_7119281
_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         'C42 H36 N4 O, 2(C2 H6 O S)'
_chemical_formula_sum            'C46 H48 N4 O3 S2'
_chemical_formula_weight         769.00
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-04
_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                78.582(4)
_cell_angle_beta                 80.858(4)
_cell_angle_gamma                89.827(4)
_cell_formula_units_Z            2
_cell_length_a                   9.7749(4)
_cell_length_b                   10.2099(4)
_cell_length_c                   21.6219(10)
_cell_measurement_reflns_used    17746
_cell_measurement_temperature    200
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      2.03
_cell_volume                     2087.41(16)
_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    'Diamond 2/3, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'MS Word, Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'image plate (34cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE image plate'
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.917
_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  0.0613
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_Laue_measured_fraction_full 0.936
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            18610
_diffrn_reflns_point_group_measured_fraction_full 0.936
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.278
_diffrn_reflns_theta_min         2.036
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  0.8579
_exptl_absorpt_correction_T_min  0.5624
_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    1.223
_exptl_crystal_description       prism
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.531
_exptl_crystal_size_mid          0.306
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         9492
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0954P)^2^+0.3598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1686
_refine_ls_wR_factor_ref         0.1809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7220
_reflns_number_total             9492
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc08958e2.cif
_cod_data_source_block           pTolylLDBFH2
_cod_depositor_comments
'Adding full bibliography for 7119278--7119283.cif.'
_cod_database_code               7119281
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Others
 Fixed Sof: S2A(0.8) S2B(0.2) H45A(0.8) H45B(0.8) H45C(0.8) H45D(0.2)
 H45E(0.2) H45F(0.2) H46A(0.8) H46B(0.8) H46C(0.8) H46D(0.2) H46E(0.2)
 H46F(0.2) S1A(0.85) S1B(0.15) H43A(0.85) H43B(0.85) H43C(0.85) H43D(0.15)
 H43E(0.15) H43F(0.15) H44A(0.85) H44B(0.85) H44C(0.85) H44D(0.15) H44E(0.15)
 H44F(0.15)
3.a Me refined with riding coordinates:
 C45(H45A,H45B,H45C), C45(H45D,H45E,H45F), C46(H46A,H46B,H46C), C46(H46D,H46E,
 H46F), C43(H43A,H43B,H43C), C43(H43D,H43E,H43F), C44(H44A,H44B,H44C), C44(H44D,
 H44E,H44F)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C16(H16), C17(H17),
 C19(H19), C20(H20), C23(H23), C24(H24), C26(H26), C27(H27), C30(H30), C31(H31),
  C33(H33), C34(H34), C37(H37), C38(H38), C40(H40), C41(H41)
3.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C28(H28A,H28B,H28C), C35(H35A,H35B,H35C), C42(H42A,H42B,
 H42C)
;
_shelx_res_checksum              1274
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'