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_1571458
_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         'C36 H50 N7 P S2'
_chemical_formula_sum            'C36 H50 N7 P S2'
_chemical_formula_weight         675.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-06-24 deposited with the CCDC.	2024-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.208(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3245(15)
_cell_length_b                   18.881(3)
_cell_length_c                   17.927(2)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    272.0
_cell_measurement_theta_max      54.915
_cell_measurement_theta_min      4.535
_cell_volume                     3793.8(9)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      272.0
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0591
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36147
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        24.990
_diffrn_reflns_theta_max         24.990
_diffrn_reflns_theta_min         2.006
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1189 before and 0.0605 after correction.
The Ratio of minimum to maximum transmission is 0.8476.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         6578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_gt           0.0671
_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^)+(0.0724P)^2^+1.6599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1720
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4100
_reflns_number_total             6578
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3py01231j2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1571457--1571458.cif.'
_cod_original_cell_volume        3794.0(9)
_cod_database_code               1571458
_shelx_shelxl_version_number     2018/3
_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.a Ternary CH refined with riding coordinates:
 C00K(H00K), C00N(H00N), C00Q(H00Q), C00T(H00T)
2.b Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00O(H00O), C00P(H00P), C00R(H00R), C00U(H00U), C00W(H00W),
 C00X(H00X), C012(H012), C013(H013), C014(H014)
2.c Idealised Me refined as rotating group:
 C00S(H00A,H00B,H00C), C00V(H00D,H00E,H00F), C00Y(H00G,H00I,H00J), C00Z(H00L,
 H00M,H00S), C010(H01A,H01B,H01C), C011(H01D,H01E,H01F), C015(H01G,H01H,H01I),
 C016(H01J,H01K,H01L), C017(H01M,H01N,H01O), C018(H01P,H01Q,H01R), C019(H01S,
 H01T,H01U), C01A(H01V,H01W,H01X)
;
_shelx_res_checksum              23561
_olex2_submission_special_instructions 'No special instructions were received'