Visible-light-induced synthesis of polymers with versatile end groups mediated by organocobalt complexes
Liu, Xu; Tian, Lei; Wu, Zhenqiang; Zhao, Xianyuan; Wang, Zikuan; Yu, Donggeng; Fu, Xuefeng; Polym. Chem.  (2017) –; doi:10.1039/C7PY01086A

data_1546770
_publ_section_title
;
 Visible-light-induced synthesis of polymers with versatile end groups
 mediated by organocobalt complexes
;
_journal_name_full               'Polym. Chem.'
_journal_paper_doi               10.1039/C7PY01086A
_journal_year                    2017
_chemical_formula_moiety         'C45 H68 Co N3 O3'
_chemical_formula_sum            'C45 H68 Co N3 O3'
_chemical_formula_weight         757.95
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-17
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-10-18 deposited with the CCDC.
2017-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.313(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.383(3)
_cell_length_b                   10.7067(18)
_cell_length_c                   23.844(4)
_cell_measurement_reflns_used    13751
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4851
_cell_measurement_theta_min      1.5043
_cell_volume                     4182.4(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  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2014)'
_computing_structure_solution
;
'SHELXT (Sheldrick, 2014)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 45.0721
              2theta: -19.8549
scan:
    Number of images: 270
               Slice: -76.2500 - 58.7500
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 45.0721
              2theta: -19.8549
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0526
_diffrn_orient_matrix_UB_12      0.0293
_diffrn_orient_matrix_UB_13      -0.0100
_diffrn_orient_matrix_UB_21      0.0142
_diffrn_orient_matrix_UB_22      -0.0515
_diffrn_orient_matrix_UB_23      -0.0766
_diffrn_orient_matrix_UB_31      -0.0201
_diffrn_orient_matrix_UB_32      0.0287
_diffrn_orient_matrix_UB_33      -0.0230
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            29483
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.107
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.452
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       block
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.253
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         9525
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.253
_refine_ls_R_factor_all          0.1290
_refine_ls_R_factor_gt           0.1231
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+27.5298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2472
_refine_ls_wR_factor_ref         0.2500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8853
_reflns_number_total             9525
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7py01086a2.cif
_cod_data_source_block           mx3858
_cod_original_cell_volume        4182.3(12)
_cod_database_code               1546770
_diffrn_number_total             10024
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C39-C38 = C39A-C38
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C39 \\sim C39A \\sim C38 \\sim O3A \\sim O3: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(C4A) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(H3BC)=Sof(H3BD)=Sof(H6BC)=Sof(H6BD)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C4A)=
 Sof(H4AA)=Sof(H4AB)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=1-FVAR(1)
 Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(H3AA)=Sof(H3AB)=Sof(C4)=Sof(H4A)=Sof(H4B)=
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H6AA)=Sof(H6AB)=FVAR(1)
 Sof(H38A)=Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=Sof(O3A)=1-FVAR(2)
 Sof(O3)=Sof(H38)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C38(H38), C38(H38A), C40(H40), C1A(H1A), C2A(H2A)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3AA,H3AB), C3(H3BC,H3BD), C4(H4A,H4B), C5(H5A,H5B), C6(H6AA,H6AB),
 C6(H6BC,H6BD), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B),
 C45(H45A,H45B), C5A(H5AA,H5AB), C4A(H4AA,H4AB)
5.c Aromatic/amide H refined with riding coordinates:
 N3(H3), C7(H7), C9(H9), C11(H11), C22(H22), C24(H24), C26(H26)
5.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C), C39(H39A,H39B,H39C), C39A(H39D,H39E,H39F)
;
_shelx_res_checksum              56433
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'