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_7121453
_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 N8 P4 Sm2, 0.5(C7 H8)'
_chemical_formula_sum            'C103.5 H144 N8 P4 Sm2'
_chemical_formula_weight         1924.84
_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                98.3430(10)
_cell_angle_beta                 96.4380(10)
_cell_angle_gamma                111.5060(10)
_cell_formula_units_Z            2
_cell_length_a                   14.1425(2)
_cell_length_b                   14.9026(2)
_cell_length_c                   26.1273(4)
_cell_measurement_reflns_used    52605
_cell_measurement_temperature    110
_cell_measurement_theta_max      30.17
_cell_measurement_theta_min      1.55
_cell_volume                     4986.58(13)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.127.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.71.0.0 (STOE, 2016)
X-Area X-Red32 1.63.2.0 (STOE, 2017) 
;
_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      110.0
_diffrn_detector                 Pilatus100K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 100K'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            43509
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.082
_diffrn_reflns_theta_min         1.551
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.279
_exptl_absorpt_correction_T_max  0.8783
_exptl_absorpt_correction_T_min  0.7127
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE XRed & XShape'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       prism
_exptl_crystal_F_000             2010
_exptl_crystal_recrystallization_method
'The material was recrystallised from toluene by slow evaporation'
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.218
_refine_diff_density_max         1.429
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1108
_refine_ls_number_reflns         19417
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0438P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0737
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15993
_reflns_number_total             19417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01519h2.cif
_cod_data_source_block           csp140
_cod_depositor_comments
'Adding full bibliography for 7121453--7121456.cif.'
_cod_original_formula_sum        'C103.50 H144 N8 P4 Sm2'
_cod_database_code               7121453
_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. Restrained distances
 C1A-C1B
 1.51 with sigma of 0.02
 C1B-C1C \\sim C1C-C1D \\sim C1D-C1E \\sim C1E-C1F \\sim C1F-C1G \\sim C1G-C1B
 with sigma of 0.02
 C1B-C1F \\sim C1B-C1D \\sim C1G-C1E \\sim C1C-C1G \\sim C1D-C1F \\sim C1C-C1E
 with sigma of 0.04
 C1A-C1G \\sim C1A-C1C
 with sigma of 0.04
3. Restrained planarity
 C1A, C1B, C1C, C1D, C1E, C1F, C1G
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C1A \\sim C1B \\sim C1C \\sim C1D \\sim C1E \\sim C1F \\sim C1G: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C1A, C1B, C1C, C1D, C1E, C1F, C1G
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C1B(0.5) C1C(0.5) H1C(0.5)
 C1D(0.5) H1D(0.5) C1E(0.5) H1E(0.5) C1F(0.5) H1F(0.5) C1G(0.5) H1G(0.5)
7.a Free rotating group:
 C1A(C1B,C1C,C1D,C1E,C1F,C1G)
7.b Ternary CH refined with riding coordinates:
 C58(H58), C73(H73), C33(H33), C95(H95), C36(H36), C23(H23), C20(H20),
 C98(H98), C83(H83), C11(H11), C8(H8), C61(H61), C86(H86), C45(H45), C70(H70),
 C48(H48)
7.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C18(H18), C4(H4), C31(H31), C51(H51), C91(H91), C80(H80), C1(H1),
 C92(H92), C56(H56), C76(H76), C26(H26), C79(H79), C66(H66), C93(H93), C68(H68),
  C43(H43), C67(H67), C54(H54), C81(H81), C29(H29), C55(H55), C5(H5), C42(H42),
 C30(H30), C41(H41), C17(H17), C6(H6), C1C(H1C), C1D(H1D), C1E(H1E), C1F(H1F),
 C1G(H1G)
7.d Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C), C13(H13A,H13B,H13C), C22(H22A,H22B,H22C), C72(H72A,H72B,
 H72C), C25(H25A,H25B,H25C), C21(H21A,H21B,H21C), C99(H99A,H99B,H99C), C59(H59A,
 H59B,H59C), C46(H46A,H46B,H46C), C50(H50A,H50B,H50C), C60(H60A,H60B,H60C),
 C85(H85A,H85B,H85C), C37(H37A,H37B,H37C), C75(H75A,H75B,H75C), C34(H34A,H34B,
 H34C), C87(H87A,H87B,H87C), C62(H62A,H62B,H62C), C10(H10A,H10B,H10C), C71(H71A,
 H71B,H71C), C47(H47A,H47B,H47C), C97(H97A,H97B,H97C), C96(H96A,H96B,H96C),
 C12(H12A,H12B,H12C), C9(H9A,H9B,H9C), C35(H35A,H35B,H35C), C74(H74A,H74B,H74C),
  C49(H49A,H49B,H49C), C84(H84A,H84B,H84C), C24(H24A,H24B,H24C), C88(H88A,H88B,
 H88C), C100(H10D,H10E,H10F), C38(H38A,H38B,H38C), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              98736
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop oil'
_olex2_submission_special_instructions 'No special instructions were received'