N,N′-Bis(imidazolyl)guanidinylphosphines: powerful initiators for conjugate-addition polymerization of Michael-type monomers
Wen, Lang-Qi; Chen, Wei; Ren, Wei-Min; Lu, Xiao-Bing; Zhou, Hui; Polymer Chemistry 15 (2024) 1877–1883; doi:10.1039/D3PY01231J

data_1571457
_publ_section_title
;
 N,N&#x2032;-Bis(imidazolyl)guanidinylphosphines: powerful initiators for
 conjugate-addition polymerization of Michael-type monomers
;
_journal_issue                   18
_journal_name_full               'Polymer Chemistry'
_journal_page_first              1877
_journal_page_last               1883
_journal_paper_doi               10.1039/D3PY01231J
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C35 H62 N7 P'
_chemical_formula_sum            'C35 H62 N7 P'
_chemical_formula_weight         611.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2bn5hp
_audit_creation_date             2020-12-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2022-04-04 deposited with the CCDC.	2024-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.677(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1956(5)
_cell_length_b                   16.7938(7)
_cell_length_c                   21.6192(10)
_cell_measurement_reflns_used    7190
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      22.883
_cell_measurement_theta_min      2.327
_cell_volume                     4051.2(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1430
_diffrn_reflns_av_unetI/netI     0.0865
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            49880
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.191
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1358 before and 0.0721 after correction.
The Ratio of minimum to maximum transmission is 0.7391.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.003
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         7117
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1179
_refine_ls_R_factor_gt           0.0661
_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^)+(0.1084P)^2^+0.5746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1802
_refine_ls_wR_factor_ref         0.2055
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4199
_reflns_number_total             7117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3py01231j2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1571457--1571458.cif.'
_cod_database_code               1571457
_shelx_shelxl_version_number     2018/3
_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. Uiso/Uaniso restraints and constraints
Uanis(C19) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C15A) \\sim Ueq,
Uanis(C27A) \\sim Ueq, Uanis(C33A) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C3A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 P1, C2, C2A, C3, C3A, C15, C15A, C19, C27, C27A, C33, C33A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C15A)=Sof(H15C)=
 Sof(H15D)=Sof(H19A)=Sof(C27A)=Sof(H27C)=Sof(H27D)=Sof(C33A)=Sof(H33C)=
 Sof(H33D)=1-FVAR(1)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C15)=Sof(H15A)=
 Sof(H15B)=Sof(H19)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C33)=Sof(H33A)=Sof(H33B)=
 FVAR(1)
 Fixed Sof: C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C17A(0.5) H17D(0.5)
 H17E(0.5) H17F(0.5) H28(0.5) H28A(0.5)
5.a Ternary CH refined with riding coordinates:
 C6(H6), C12(H12), C19(H19), C19(H19A), C20(H20), C28(H28), C28(H28A), C32(H32)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C2A(H2AA,H2AB), C3(H3A,H3B), C3A(H3AA,H3AB), C11(H11A,H11B),
 C13(H13A,H13B), C15(H15A,H15B), C15A(H15C,H15D), C26(H26A,H26B), C27(H27A,
 H27B), C27A(H27C,H27D), C29(H29A,H29B), C33(H33A,H33B), C33A(H33C,H33D),
 C34(H34A,H34B)
5.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C),
 C17A(H17D,H17E,H17F), C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C35(H35A,H35B,H35C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              96288
_shelx_fab_checksum              3769
_olex2_submission_special_instructions 'No special instructions were received'