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_7121455
_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         'C100 H140 As4 N8 Sm2'
_chemical_formula_sum            'C100 H140 As4 N8 Sm2'
_chemical_formula_weight         2054.57
_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
_audit_creation_date             2017-03-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2018-01-22 deposited with the CCDC.
2018-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                99.664(4)
_cell_angle_beta                 94.939(4)
_cell_angle_gamma                95.996(4)
_cell_formula_units_Z            2
_cell_length_a                   13.6808(7)
_cell_length_b                   16.1681(8)
_cell_length_c                   22.4917(11)
_cell_measurement_reflns_used    25562
_cell_measurement_temperature    110
_cell_measurement_theta_max      29.84
_cell_measurement_theta_min      1.29
_cell_volume                     4850.2(4)
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2008)'
_diffrn_ambient_temperature      108.0
_diffrn_detector                 Pilatus100K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_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  0.0616
_diffrn_reflns_av_unetI/netI     0.0794
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            44165
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.097
_diffrn_reflns_theta_min         1.287
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.601
_exptl_absorpt_correction_T_max  0.9199
_exptl_absorpt_correction_T_min  0.7714
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE XRed & STOE XShape'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       plate
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.144
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.03
_refine_diff_density_max         5.192
_refine_diff_density_min         -1.334
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1059
_refine_ls_number_reflns         19049
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0909P)^2^+10.5113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.1755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12156
_reflns_number_total             19049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01519h2.cif
_cod_data_source_block           csp181
_cod_depositor_comments
'Adding full bibliography for 7121453--7121456.cif.'
_cod_database_code               7121455
_shelx_shelxl_version_number     2016/6
_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:
 C98(H98), C45(H45), C61(H61), C36(H36), C83(H83), C59(H59), C95(H95), C9(H9),
 C23(H23), C8(H8), C33(H33), C70(H70), C20(H20), C86(H86), C73(H73), C48(H48)
2.b Aromatic/amide H refined with riding coordinates:
 C67(H67), C16(H16), C66(H66), C51(H51), C92(H92), C43(H43), C80(H80),
 C76(H76), C29(H29), C26(H26), C56(H56), C4(H4), C93(H93), C81(H81), C55(H55),
 C79(H79), C5(H5), C18(H18), C31(H31), C42(H42), C1(H1), C91(H91), C30(H30),
 C17(H17), C41(H41), C68(H68), C54(H54), C6(H6)
2.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C47(H47A,H47B,H47C), C10(H10A,H10B,H10C), C50(H50A,H50B,
 H50C), C100(H10D,H10E,H10F), C62(H62A,H62B,H62C), C96(H96A,H96B,H96C),
 C71(H71A,H71B,H71C), C99(H99A,H99B,H99C), C37(H37A,H37B,H37C), C46(H46A,H46B,
 H46C), C49(H49A,H49B,H49C), C85(H85A,H85B,H85C), C58(H58A,H58B,H58C), C21(H21A,
 H21B,H21C), C35(H35A,H35B,H35C), C75(H75A,H75B,H75C), C74(H74A,H74B,H74C),
 C22(H22A,H22B,H22C), C60(H60A,H60B,H60C), C84(H84A,H84B,H84C), C25(H25A,H25B,
 H25C), C24(H24A,H24B,H24C), C12(H12A,H12B,H12C), C34(H34A,H34B,H34C), C72(H72A,
 H72B,H72C), C88(H88A,H88B,H88C), C13(H13A,H13B,H13C), C11(H11A,H11B,H11C),
 C87(H87A,H87B,H87C), C63(H63A,H63B,H63C), C97(H97A,H97B,H97C)
;
_shelx_res_checksum              43348
_olex2_submission_special_instructions 'No special instructions were received'