Phosphine-functionalized amidinate ligated rare-earth metal complexes for highly 3,4-selective living polymerization of 1,3-conjugated dienes.
You, Fen; Wang, Jixing; Liu, Hui; Kang, Xiaohui; Shi, Xiaochao; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d2dt04167g

data_7713552
_publ_section_title
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 Phosphine-functionalized amidinate ligated rare-earth metal complexes for
 highly 3,4-selective living polymerization of 1,3-conjugated dienes.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d2dt04167g
_journal_year                    2023
_chemical_formula_moiety         'C51 H58 N4 P Sc'
_chemical_formula_sum            'C51 H58 N4 P Sc'
_chemical_formula_weight         802.94
_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
_audit_block_doi                 10.5517/ccdc.csd.cc2fx09p
_audit_creation_date             2023-05-06
_audit_creation_method
; 
Olex2 1.2-beta 
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103) 
;
_audit_update_record
;
2023-05-07 deposited with the CCDC.	2023-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                89.192(4)
_cell_angle_beta                 71.996(4)
_cell_angle_gamma                87.743(4)
_cell_formula_units_Z            2
_cell_length_a                   11.8185(12)
_cell_length_b                   12.4335(15)
_cell_length_c                   15.9472(17)
_cell_measurement_reflns_used    2373
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.13
_cell_measurement_theta_min      2.49
_cell_volume                     2226.9(4)
_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    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1220
_diffrn_reflns_av_unetI/netI     0.2026
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13826
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.150
_diffrn_reflns_theta_max         25.150
_diffrn_reflns_theta_min         1.894
_exptl_absorpt_coefficient_mu    0.240
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5296
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1162 before and 0.0839 after correction. 
The Ratio of minimum to maximum transmission is 0.7103. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       0.044(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         7945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1831
_refine_ls_R_factor_gt           0.0955
_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^)+(0.1298P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2159
_refine_ls_wR_factor_ref         0.2731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3934
_reflns_number_total             7945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04167g2.cif
_cod_data_source_block           mo_230322c
_cod_database_code               7713552
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.990
_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: 
 C22(H22), C25(H25) 
2.b Secondary CH2 refined with riding coordinates: 
 C2(H2A,H2B), C3(H3A,H3B) 
2.c Aromatic/amide H refined with riding coordinates: 
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13), 
 C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C29(H29), C30(H30), C31(H31), 
  C32(H32), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39), C40(H40), 
 C43(H43), C46(H46), C47(H47), C48(H48), C49(H49) 
2.d Idealised Me refined as rotating group: 
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B, 
 H27C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C50(H50A,H50B,H50C), C51(H51A, 
 H51B,H51C) 
;
_shelx_res_checksum              32508
_shelx_shelxl_version_number     2019/2
_olex2_submission_special_instructions 'No special instructions were received'