A well-defined, versatile photoinitiator (salen)Co‒CO2CH3for visible light-initiated living/controlled radical polymerization
Zhao, Yaguang; Yu, Mengmeng; Zhang, Shuailin; Wu, Zhenqiang; Liu, Yuchu; Peng, Chi-How; Fu, Xuefeng; Chem. Sci. 6 (2015) 2979–; doi:10.1039/C5SC00477B

data_1518782
_publ_section_title
;
 A well-defined, versatile photoinitiator (salen)Co--CO2CH3for visible
 light-initiated living/controlled radical polymerization
;
_journal_issue                   5
_journal_name_full               'Chem. Sci.'
_journal_page_first              2979
_journal_paper_doi               10.1039/C5SC00477B
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C38 H55 Co N2 O4'
_chemical_formula_sum            'C38 H55 Co N2 O4'
_chemical_formula_weight         662.77
_chemical_name_systematic        (salen)Co-CO2CH3
_chemical_properties_physical    'Heat-sensitive, Light-sensitive'
_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   geom
_audit_creation_date             2014-02-11
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_audit_update_record
;
2014-10-27 deposited with the CCDC.
2015-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.629(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.569(4)
_cell_length_b                   10.302(2)
_cell_length_c                   19.781(4)
_cell_measurement_reflns_used    11364
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4812
_cell_measurement_theta_min      1.9769
_cell_volume                     3518.8(13)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
'XS (Sheldrick, 2008)' 
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0061
_diffrn_orient_matrix_UB_12      0.0512
_diffrn_orient_matrix_UB_13      -0.0264
_diffrn_orient_matrix_UB_21      0.0714
_diffrn_orient_matrix_UB_22      -0.0367
_diffrn_orient_matrix_UB_23      -0.0546
_diffrn_orient_matrix_UB_31      -0.0328
_diffrn_orient_matrix_UB_32      -0.0055
_diffrn_orient_matrix_UB_33      -0.0392
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23869
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.492
_diffrn_reflns_theta_min         2.359
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.529
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/hexane'
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.927
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.260
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         8036
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.257
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0698
_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^)+(0.0235P)^2^+8.3213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1519
_refine_ls_wR_factor_ref         0.1534
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7717
_reflns_number_total             8036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc00477b2.cif
_cod_data_source_block           sa3204
_cod_depositor_comments          'Adding full bibliography for 1518782.cif.'
_cod_original_cell_volume        3518.8(12)
_cod_database_code               1518782
_shelxl_version_number           2013-4
_diffrn_number_total             8495
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C25A)
\\sim Ueq, Uanis(C24A) \\sim Ueq, Uanis(C26A) \\sim Ueq, Uanis(C33A) \\sim Ueq,
Uanis(C34A) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C37A)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C36A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(H35C)=Sof(H35D)=Sof(H38C)=Sof(H38D)=Sof(C37A)=Sof(H37C)=Sof(H37D)=
 Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C34A)=Sof(H34A)=Sof(C33A)=Sof(H33A)=1-FVAR(1)
 Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34)=Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36A)=
 Sof(H36B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H38A)=Sof(H38B)=FVAR(1)
 Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C24A)=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(2)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C33(H33), C34(H34), C34A(H34A), C33A(H33A)
4.b Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C35(H35C,H35D), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,
 H38B), C38(H38C,H38D), C37A(H37C,H37D), C36A(H36C,H36D)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C7(H7), C16(H16), C18(H18), C20(H20)
4.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C25A(H25D,H25E,H25F), C24A(H24D,H24E,
 H24F), C26A(H26D,H26E,H26F)
;
_shelx_res_checksum              64002