Room Temperature Multicomponent Polymerizations of Alkynes, Sulfonyl Azides, and Iminophosphorane toward Heteroatom-Rich Multifunctional Poly(phosphorus amidine)s
Xu, Liguo; Hu, Rongrong; Tang, Ben Zhong; Macromolecules 50 (2017) 6043–; doi:10.1021/acs.macromol.7b01096

data_1546987
_publ_section_title
;
 Room Temperature Multicomponent Polymerizations of Alkynes, Sulfonyl
 Azides, and Iminophosphorane toward Heteroatom-Rich Multifunctional
 Poly(phosphorus amidine)s
;
_journal_issue                   16
_journal_name_full               Macromolecules
_journal_page_first              6043
_journal_paper_doi               10.1021/acs.macromol.7b01096
_journal_volume                  50
_journal_year                    2017
_chemical_formula_moiety         'C39 H33 N2 O2 P S'
_chemical_formula_sum            'C39 H33 N2 O2 P S'
_chemical_formula_weight         624.70
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-07-05
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                104.914(7)
_cell_angle_beta                 97.452(6)
_cell_angle_gamma                113.494(7)
_cell_formula_units_Z            2
_cell_length_a                   10.9011(7)
_cell_length_b                   12.3189(10)
_cell_length_c                   13.9641(10)
_cell_measurement_reflns_used    2825
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.2321
_cell_measurement_theta_min      3.1224
_cell_volume                     1603.7(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0633532000
_diffrn_orient_matrix_UB_12      0.0433447000
_diffrn_orient_matrix_UB_13      0.0373264000
_diffrn_orient_matrix_UB_21      -0.0097886000
_diffrn_orient_matrix_UB_22      -0.0432607000
_diffrn_orient_matrix_UB_23      0.0267989000
_diffrn_orient_matrix_UB_31      0.0359939000
_diffrn_orient_matrix_UB_32      -0.0265746000
_diffrn_orient_matrix_UB_33      -0.0292488000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10059
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.13
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.189
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         5858
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+0.1615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1394
_reflns_number_gt                4150
_reflns_number_total             5858
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ma7b01096_si_002.cif
_cod_data_source_block           160705_xlg_22
_cod_database_code               1546987
_chemical_oxdiff_formula         'c10 h10 n2 o8 p1 s1'
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C29(H29), C35(H35), C5(H5), C6(H6), C15(H15), C39(H39), C21(H21),
 C11(H11), C3(H3), C12(H12), C32(H32), C13(H13), C2(H2A), C33(H33), C14(H14),
 C30(H30), C36(H36), C17(H17), C31(H31), C38(H38), C23(H23), C25(H25), C27(H27),
  C37(H37), C20(H20), C24(H24), C18(H18), C26(H26), C19(H19)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;