Reactivity of Mixed Methyl-Aminobenzyl Guanidinate Lutetium Complex towards iPrN=C=NiPr, CS2 and Ph2PH
Jiang, Wen; Zhang, Lijun; Zhang, Lixin; Dalton Transactions  (2022) –; doi:10.1039/D2DT02008D

data_7710839
_publ_section_title
;
 Reactivity of Mixed Methyl-Aminobenzyl Guanidinate Lutetium Complex
 towards iPrN=C=NiPr, CS2 and Ph2PH
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02008D
_journal_year                    2022
_chemical_formula_moiety         'C142 H168 Lu2 N6 O4 P4'
_chemical_formula_sum            'C142 H168 Lu2 N6 O4 P4'
_chemical_formula_weight         2496.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-07-26 deposited with the CCDC.	2022-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                85.697(4)
_cell_angle_beta                 70.525(4)
_cell_angle_gamma                77.353(4)
_cell_formula_units_Z            1
_cell_length_a                   14.5232(14)
_cell_length_b                   15.3348(15)
_cell_length_c                   15.5621(15)
_cell_measurement_reflns_used    9845
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      56.88
_cell_measurement_theta_min      3.43
_cell_volume                     3188.3(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      172.98
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0916
_diffrn_reflns_av_unetI/netI     0.0788
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            48926
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         57.497
_diffrn_reflns_theta_min         3.194
_exptl_absorpt_coefficient_mu    2.534
_exptl_absorpt_correction_T_max  0.5795
_exptl_absorpt_correction_T_min  0.4420
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.507
_refine_diff_density_min         -1.122
_refine_diff_density_rms         0.207
_refine_ls_extinction_coef       0.0124(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         13112
_refine_ls_number_restraints     408
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.1190
_refine_ls_R_factor_gt           0.1008
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2775
_refine_ls_wR_factor_ref         0.2923
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9980
_reflns_number_total             13112
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02008d2.cif
_cod_data_source_block           ga_90918c_a
_cod_database_code               7710839
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.804
_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. Restrained distances
 P1-C49'
 2.8 with sigma of 0.05
 P1-C44'
 1.8 with sigma of 0.02
 C17-C18 = C18-C19 = C46-C47 = C47-C48 = C48-C49 = C58-C59
 1.4 with sigma of 0.02
 C52-C53 = C54-C55 = C61-C62 = C62-C63 = C68-C69 = C69-C70
 1.4 with sigma of 0.02
3. Rigid bond restraints
 P1, C44'
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C53, C54, C55
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C46 \\sim C47 \\sim C48 \\sim C49 \\sim C46' \\sim C47' \\sim C48' \\sim C49':
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.05
Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47)
\\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C44') \\sim Ueq,
Uanis(C45') \\sim Ueq, Uanis(C46') \\sim Ueq, Uanis(C47') \\sim Ueq,
Uanis(C48') \\sim Ueq, Uanis(C49') \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37)
\\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C52) \\sim Ueq,
Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63)
\\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C71) \\sim Ueq:
with sigma of 0.02 and sigma for terminal atoms of 0.04
5. Rigid body (RIGU) restrains
 C55, C50, C51, C52, C53, C54
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C22, C27, C26, C25, C24, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C66, C71, C70, C69, C68, C67
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C65, C64, C63, C62, C61, C60
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C51, C50, C55, C54, C53, C52
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C44(0.65) C45(0.65) H45(0.65) C46(0.65) H46(0.65) C47(0.65)
 H47(0.65) C48(0.65) H48(0.65) C49(0.65) H49(0.65) C44'(0.35) C45'(0.35)
 H45'(0.35) C46'(0.35) H46'(0.35) C47'(0.35) H47'(0.35) C48'(0.35) H48'(0.35)
 C49'(0.35) H49'(0.35)
7.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C34(H34), C37(H37)
7.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C21(H21A,H21B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,
 H42B), C43(H43A,H43B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B),
 C59(H59A,H59B)
7.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C16(H16), C20(H20), C19(H19), C18(H18), C17(H17),
 C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C30(H30), C31(H31), C32(H32),
  C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C45'(H45'), C46'(H46'),
 C47'(H47'), C48'(H48'), C49'(H49'), C51(H51), C52(H52), C53(H53), C54(H54),
 C55(H55), C65(H65), C64(H64), C63(H63), C62(H62), C61(H61), C67(H67), C68(H68),
  C69(H69), C70(H70), C71(H71)
7.d Fitted hexagon refined as free rotating group:
 C16(C15,C20,C19,C18,C17), C44'(C45',C46',C47',C48',C49'), C60(C65,C64,C63,C62,
 C61), C66(C67,C68,C69,C70,C71)
7.e Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C)
;
_olex2_submission_special_instructions 'No special instructions were received'