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_1546067
_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         'C48 H39 Cu N3 O P2, B F4, C4 H10 O'
_chemical_formula_sum            'C52 H49 B Cu F4 N3 O2 P2'
_chemical_formula_weight         960.23
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-10-23
_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                 104.764(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3268(3)
_cell_length_b                   21.2128(5)
_cell_length_c                   19.3122(5)
_cell_measurement_reflns_used    20963
_cell_measurement_temperature    293
_cell_measurement_theta_max      25.7660
_cell_measurement_theta_min      3.7790
_cell_volume                     4883.1(2)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_details
;
  1 omega  -20.00   33.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.0735  -99.0000 -150.0000 53

  2 omega  -19.00   84.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       10.1672   57.0000   60.0000 103

  3 omega  -16.00   86.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       10.1672   38.0000  -30.0000 102

  4 omega  -16.00   86.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       10.1672   38.0000 -150.0000 102

  5 omega  -19.00   84.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       10.1672   57.0000  150.0000 103

  6 omega   14.00   82.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       10.1672 -148.0000 -133.0000 68

  7 omega  -20.00    5.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       10.1672  -99.0000  -90.0000 25

  8 omega    1.00   67.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       10.1672 -124.0000   30.0000 66
;
_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      0.0365763000
_diffrn_orient_matrix_UB_12      0.0111878000
_diffrn_orient_matrix_UB_13      0.0321858000
_diffrn_orient_matrix_UB_21      -0.0168759000
_diffrn_orient_matrix_UB_22      0.0313910000
_diffrn_orient_matrix_UB_23      -0.0099361000
_diffrn_orient_matrix_UB_31      -0.0437878000
_diffrn_orient_matrix_UB_32      -0.0027560000
_diffrn_orient_matrix_UB_33      0.0175585000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            74466
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.686
_diffrn_reflns_theta_min         3.350
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.571
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85418
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       prism
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         11275
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0760P)^2^+5.2416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1496
_refine_ls_wR_factor_ref         0.1650
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8488
_reflns_number_total             11275
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7py00726d2.cif
_cod_data_source_block           ank128
_cod_database_code               1546067
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'c48 h39 b1 cu1 f4 n3 o1 p2'
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-C51
 1.4 with sigma of 0.01
 O2-C49
 1.4 with sigma of 0.01
 C49-C50
 1.5 with sigma of 0.01
 C51-C52
 1.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(F2) = Uanis(F3) = Uanis(F4) = Uanis(F6) = Uanis(F5) = Uanis(F7)
4. Others
 Sof(F5)=Sof(F6)=Sof(F7)=1-FVAR(1)
 Sof(F2)=Sof(F3)=Sof(F4)=FVAR(1)
5.a Rotating group:
 N3(H3A,H3B)
5.b Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C51(H51A,H51B)
5.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),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22),
  C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C32(H32),
 C33(H33), C34(H34), C35(H35), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
  C44(H44), C45(H45), C46(H46), C47(H47), C48(H48)
5.d Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C52(H52A,H52B,H52C)
;
_olex2_submission_special_instructions 'No special instructions were received'