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_7713553
_publ_section_title
;
 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         'C52 H62 N4 P Sc, 0.35[C6H14], 0.275[C6H14]'
_chemical_formula_sum            'C55.75 H70.75 N4 P Sc'
_chemical_formula_weight         872.84
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2dsdcz
_audit_creation_date             2023-07-14
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-07-14 deposited with the CCDC.	2023-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                93.267(3)
_cell_angle_beta                 90.002(4)
_cell_angle_gamma                101.270(3)
_cell_formula_units_Z            4
_cell_length_a                   11.8911(6)
_cell_length_b                   15.1281(7)
_cell_length_c                   27.9116(14)
_cell_measurement_reflns_used    4075
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      66.44
_cell_measurement_theta_min      3.17
_cell_volume                     4915.9(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1409
_diffrn_reflns_av_unetI/netI     0.1082
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            72491
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.849
_diffrn_reflns_theta_max         66.849
_diffrn_reflns_theta_min         1.585
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.882
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6089
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1309 before and 0.0768 after correction.
The Ratio of minimum to maximum transmission is 0.8088.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_description       block
_exptl_crystal_F_000             1877
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1061
_refine_ls_number_reflns         17382
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0712P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1481
_refine_ls_wR_factor_ref         0.1677
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11176
_reflns_number_total             17382
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04167g2.cif
_cod_data_source_block           sc_a
_cod_database_code               7713553
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.912
_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:
 C014(H014), C01D(H01D), C32(H32), C35(H35)
2.b Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C00K(H00A,H00B), C00L(H00C,H00D), C39(H39A,H39B), C011(H01A,
 H01B), C38(H38A,H38B), C01H(H01E,H01F), C01K(H01G,H01H), C1(H1A,H1B), C10(H10A,
 H10B)
2.c Aromatic/amide H refined with riding coordinates:
 C46(H46), C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C42(H42),
 C010(H010), C012(H012), C015(H015), C48(H48), C45(H45), C44(H44), C21(H21),
 C01C(H01C), C22(H22), C25(H25), C01J(H01J), C01M(H01M), C01N(H01N), C01S(H01S),
  C01U(H01U), C15(H15), C43(H43), C020(H020), C24(H24), C6(H6), C4(H4), C3(H3),
 C5(H5), C029(H029), C23(H23), C14(H14), C02G(H02G), C02H(H02H), C02I(H02I),
 C02J(H02J), C02L(H02L), C49(H49), C02Q(H02R), C02R(H02S), C02S(H02T), C12(H12),
  C02V(H02X), C52(H52), C13(H13), C50(H50), C030(H030), C031(H031), C51(H51),
 C30(H30), C28(H28), C29(H29)
2.d Idealised Me refined as rotating group:
 C01Q(H01I,H01K,H01L), C01R(H01O,H01P,H01Q), C17(H17A,H17B,H17C), C023(H02A,
 H02B,H02C), C026(H02D,H02E,H02F), C36(H36A,H36B,H36C), C18(H18A,H18B,H18C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C02N(H02K,H02M,H02N), C02P(H02O,H02P,
 H02Q), C02U(H02U,H02V,H02W), C02X(H02Y,H,HA), C8(H8A,H8B,H8C), C37(H37A,H37B,
 H37C), C9(H9A,H9B,H9C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              64316
_shelx_fab_checksum              16847
_olex2_submission_special_instructions 'No special instructions were received'