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_1546767
_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_absolute_configuration ad
_chemical_formula_moiety         'C36 H52 Co N2 O2, 0.5(C H Cl3)'
_chemical_formula_sum            'C36.5 H52.5 Cl1.5 Co N2 O2'
_chemical_formula_weight         663.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-05-27
_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
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.1542(10)
_cell_length_b                   26.460(3)
_cell_length_c                   26.744(3)
_cell_measurement_reflns_used    20840
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4778
_cell_measurement_theta_min      1.0826
_cell_volume                     7185.6(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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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: 270.0000
                 XTD: 45.0056
              2theta: -20.1895
;
_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      -0.0015
_diffrn_orient_matrix_UB_12      0.0945
_diffrn_orient_matrix_UB_13      0.0275
_diffrn_orient_matrix_UB_21      -0.0267
_diffrn_orient_matrix_UB_22      0.0071
_diffrn_orient_matrix_UB_23      -0.0258
_diffrn_orient_matrix_UB_31      -0.0264
_diffrn_orient_matrix_UB_32      -0.0078
_diffrn_orient_matrix_UB_33      0.0253
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0759
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            29857
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.477
_diffrn_reflns_theta_min         1.706
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Flack x determined using 4039 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.037(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     799
_refine_ls_number_reflns         16356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0684
_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^)+(0.0403P)^2^+5.6436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1473
_reflns_Friedel_coverage         0.812
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                13943
_reflns_number_total             16356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7py01086a2.cif
_cod_data_source_block           mx3768
_cod_depositor_comments
;

2019-03-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C36 H52 Co N2 O2), C H Cl3'
_cod_original_formula_sum        'C73 H105 Cl3 Co2 N4 O4'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1326.81
_cod_database_code               1546767
_diffrn_number_total             9067
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C16(H16), C21(H21), C16A(H16A), C21A(H21A), C37(H37)
2.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C17A(H17C,
 H17D), C18A(H18C,H18D), C19A(H19C,H19D), C20A(H20C,H20D)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C15(H15), C22(H22), C24(H24), C26(H26), C3A(H3A), C5A(H5A),
 C15A(H15A), C22A(H22A), C24A(H24A), C26A(H26A)
2.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F),
 C12A(H12D,H12E,H12F), C13A(H13D,H13E,H13F), C14A(H14D,H14E,H14F), C30A(H30D,
 H30E,H30F), C31A(H31D,H31E,H31F), C32A(H32D,H32E,H32F), C34A(H34D,H34E,H34F),
 C35A(H35D,H35E,H35F), C36A(H36D,H36E,H36F)
;
_shelx_res_checksum              5006
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'