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_7119282
_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         'C28 H38 N4'
_chemical_formula_sum            'C28 H38 N4'
_chemical_formula_weight         430.62
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-20
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;
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                90
_cell_angle_beta                 114.373(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.381(3)
_cell_length_b                   8.9219(8)
_cell_length_c                   18.170(3)
_cell_measurement_reflns_used    11162
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.40
_cell_measurement_theta_min      2.12
_cell_volume                     2566.5(7)
_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 0.996
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       'two-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS2'
_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  0.0779
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16536
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.218
_diffrn_reflns_theta_min         2.115
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
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_exptl_absorpt_correction_T_min  0.9716
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_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_description       prism
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.368
_exptl_crystal_size_mid          0.307
_exptl_crystal_size_min          0.207
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         5042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0915P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1476
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3164
_reflns_number_total             5042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc08958e2.cif
_cod_data_source_block           iPrLPhenH2
_cod_depositor_comments
'Adding full bibliography for 7119278--7119283.cif.'
_cod_original_cell_volume        2566.5(6)
_cod_database_code               7119282
_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
2.a Ternary CH refined with riding coordinates:
 C17(H17), C20(H20), C23(H23), C26(H26)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C13(H13), C12(H12), C9(H9), C8(H8), C5(H5), C4(H4a), C3(H3)
2.c Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C18(H18a,H18b,H18c), C21(H21a,H21b,H21c), C22(H22a,H22b,
 H22c), C25(H25a,H25b,H25c), C24(H24a,H24b,H24c), C27(H27a,H27b,H27c), C28(H28a,
 H28b,H28c)
;
_shelx_res_checksum              39155
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'