New copper (I) complex based initiating systems in redox polymerization and comparison with amine/benzoyl peroxide reference
Lalevée, Jacques; Dietlin, Céline; Morlet-Savary, Fabrice; Fouassier, Jean Pierre; Gigmes, Didier; Dumur, Frederic; Kermagoret, Anthony; Garra, Patxi; Mousawi, Assi; Polym. Chem.  (2017) –; doi:10.1039/C7PY00726D

data_1546066
_publ_section_title
;
 New copper (I) complex based initiating systems in redox polymerization
 and comparison with amine/benzoyl peroxide reference
;
_journal_name_full               'Polym. Chem.'
_journal_paper_doi               10.1039/C7PY00726D
_journal_year                    2017
_chemical_formula_moiety         'C24 H22 Cu N6, B F4, C H2 Cl2'
_chemical_formula_sum            'C25 H24 B Cl2 Cu F4 N6'
_chemical_formula_weight         629.75
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-11-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-02-06 deposited with the CCDC.
2017-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.7581(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.15632(15)
_cell_length_b                   11.63305(16)
_cell_length_c                   22.4830(3)
_cell_measurement_reflns_used    11560
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      68.8080
_cell_measurement_theta_min      4.0870
_cell_volume                     2845.85(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -33.00   -6.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.6014  -57.0000   60.0000 27

  2 omega  -72.00  -42.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.6014  -57.0000   60.0000 30

  3 omega -106.00  -79.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.6014  -99.0000  -30.0000 27

  4 omega -117.00    3.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.6014  -57.0000  -30.0000 120

  5 omega   60.00   86.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.6014   38.0000   60.0000 26

  6 omega  105.00  131.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   77.0000   30.0000 26

  7 omega  153.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   63.0000   30.0000 25

  8 omega  152.00  177.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   77.0000   60.0000 25

  9 omega  138.00  163.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   38.0000   30.0000 25

 10 omega  139.00  177.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   32.0000  -61.0000 38

 11 omega  127.00  174.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667  111.0000 -120.0000 47

 12 omega  101.00  175.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667  111.0000 -150.0000 74

 13 omega  105.00  177.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   77.0000  -30.0000 72

 14 omega  101.00  166.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667  111.0000 -180.0000 65

 15 omega   97.00  176.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   77.0000    0.0000 79

 16 omega  103.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667  111.0000  150.0000 75

 17 omega   70.00   95.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   32.0000  -61.0000 25

 18 omega   64.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   63.0000  -30.0000 29

 19 omega   65.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   63.0000    0.0000 26

 20 omega   63.00   89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   77.0000   30.0000 26

 21 omega   68.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   50.0000    0.0000 25

 22 omega   66.00   92.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   50.0000   30.0000 26

 23 omega   64.00   90.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   38.0000   30.0000 26

 24 omega   64.00   89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   63.0000   30.0000 25

 25 omega   64.00  177.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   63.0000   60.0000 113

 26 omega   68.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   50.0000   90.0000 30

 27 omega   64.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   63.0000   90.0000 27

 28 omega   63.00   88.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   77.0000   60.0000 25

 29 omega   66.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   50.0000   60.0000 32

 30 omega   64.00  172.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   38.0000  120.0000 108

 31 omega   63.00   89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   77.0000  -30.0000 26

 32 omega   63.00   89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   77.0000    0.0000 26

 33 omega   63.00   89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667   77.0000   90.0000 26

 34 omega   17.00   83.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      104.7667  -38.0000   90.0000 66

 35 omega    6.00   59.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.6014   77.0000   30.0000 53

 36 omega  -60.00  -13.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.6014   77.0000   30.0000 47

 37 omega -123.00  -70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.6014  -57.0000   90.0000 53

 38 omega -115.00  -73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.6014 -125.0000  -90.0000 42

 39 omega -123.00  -83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.6014 -125.0000  -30.0000 40

 40 omega -124.00  -75.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.6014 -125.0000   30.0000 49

 41 omega -126.00  -80.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.6014  -99.0000   60.0000 46

 42 omega -119.00  -94.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.6014  -57.0000   60.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1331127000
_diffrn_orient_matrix_UB_12      -0.0417417000
_diffrn_orient_matrix_UB_13      -0.0056908000
_diffrn_orient_matrix_UB_21      -0.0061831000
_diffrn_orient_matrix_UB_22      -0.0353240000
_diffrn_orient_matrix_UB_23      -0.0666486000
_diffrn_orient_matrix_UB_31      0.0477837000
_diffrn_orient_matrix_UB_32      -0.1206237000
_diffrn_orient_matrix_UB_33      0.0214984000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22167
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.897
_diffrn_reflns_theta_min         4.032
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.273
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       plate
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         5244
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0722P)^2^+1.6726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1254
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4715
_reflns_number_total             5244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7py00726d2.cif
_cod_data_source_block           ank130
_cod_database_code               1546066
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'c25 h22 b1 cu1 f4 n6'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
2.a Rotating group:
 N3(H3A,H3B), N6(H6A,H6B)
2.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C20(H20), C21(H21), C23(H23),
  C24(H24)
;
_olex2_submission_special_instructions 'No special instructions were received'