Reactivity of bulky Ln(ii) amidinates towards P<sub>4</sub>, As<sub>4</sub>, and As<sub>4</sub>S<sub>4</sub>.
Schoo, Christoph; Bestgen, Sebastian; Köppe, Ralf; Konchenko, Serygey N.; Roesky, Peter W.; Chemical communications (Cambridge, England) 54 (2018) 4770–4773; doi:10.1039/c8cc01519h

data_7121454
_publ_section_title
;
 Reactivity of bulky Ln(ii) amidinates towards P<sub>4</sub>,
 As<sub>4</sub>, and As<sub>4</sub>S<sub>4</sub>.
;
_journal_issue                   38
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4770
_journal_page_last               4773
_journal_paper_doi               10.1039/c8cc01519h
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C54 H78 As N4 O S2 Sm'
_chemical_formula_sum            'C54 H78 As N4 O S2 Sm'
_chemical_formula_weight         1088.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2016-03-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-01-22 deposited with the CCDC.
2018-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.826(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6528(8)
_cell_length_b                   17.1717(7)
_cell_length_c                   21.7016(11)
_cell_measurement_reflns_used    10845
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.78
_cell_measurement_theta_min      1.52
_cell_volume                     5421.7(5)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2009)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction
'STOE X-RED & X-SHAPE, 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, 2008)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.1016
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21499
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.378
_diffrn_reflns_theta_max         25.378
_diffrn_reflns_theta_min         1.516
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.805
_exptl_absorpt_correction_T_max  0.9273
_exptl_absorpt_correction_T_min  0.8185
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE XRed & XShape'
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       needle
_exptl_crystal_F_000             2260
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         9801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0050P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0495
_refine_ls_wR_factor_ref         0.0557
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5508
_reflns_number_total             9801
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01519h2.cif
_cod_data_source_block           csp194
_cod_depositor_comments
'Adding full bibliography for 7121453--7121456.cif.'
_cod_database_code               7121454
_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.a Ternary CH refined with riding coordinates:
 C45(H45), C21(H21), C24(H24), C36(H36), C9(H9), C33(H33), C48(H48), C12(H12)
2.b Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B)
2.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C17(H17), C5(H5), C30(H30), C43(H43), C42(H42), C41(H41), C18(H18),
 C31(H31), C7(H7), C6(H6), C1(H1), C29(H29), C2(H2)
2.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C23(H23A,H23B,H23C), C34(H34A,H34B,H34C), C46(H46A,H46B,
 H46C), C49(H49A,H49B,H49C), C47(H47A,H47B,H47C), C11(H11A,H11B,H11C), C10(H10A,
 H10B,H10C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C25(H25A,H25B,H25C), C22(H22A,H22B,H22C), C35(H35A,H35B,
 H35C), C50(H50A,H50B,H50C)
;
_shelx_res_checksum              66328
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'