When cobalt-mediated [2 + 2 + 2] cycloaddition reaction dares go astray: synthesis of unprecedented cobalt(iii)-complexes.
Delorme, Marion; Punter, Alexander; Oliveira, Raquel; Aubert, Corinne; Carissan, Yannick; Parrain, Jean-Luc; Amatore, Muriel; Nava, Paola; Commeiras, Laurent; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15767–15771; doi:10.1039/c9dt03311d

data_7701169
_publ_section_title
;
 When cobalt-mediated [2 + 2 + 2] cycloaddition reaction dares go astray:
 synthesis of unprecedented cobalt(iii)-complexes.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15767
_journal_page_last               15771
_journal_paper_doi               10.1039/c9dt03311d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C28 H33 Co O6'
_chemical_formula_sum            'C28 H33 Co O6'
_chemical_formula_weight         524.47
_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             2016-08-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-07-05 deposited with the CCDC.    2019-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.2974(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.17346(17)
_cell_length_b                   15.23444(16)
_cell_length_c                   11.72199(15)
_cell_measurement_reflns_used    7679
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      65.1860
_cell_measurement_theta_min      4.3290
_cell_volume                     2441.39(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -69.00  54.00   1.00    2.00    --  -33.33  38.00   0.00  123
  2  \w   -119.00 -89.00   1.00    2.00    --  -33.33 -99.00 -90.00   30
  3  \w   -125.00-100.00   1.00    2.00    --  -33.33 -99.00   0.00   25
  4  \w    -59.00 -32.00   1.00    2.00    --  -33.33  77.00 -60.00   27
  5  \w     37.00  63.00   1.00    2.00    --  -33.33  77.00 -60.00   26
  6  \w   -123.00 -80.00   1.00    2.00    --  -33.33 -99.00 -30.00   43
  7  \w   -120.00  -2.00   1.00    2.00    --  -33.33 -57.00-120.00  118
  8  \w     29.00  66.00   1.00    2.00    --   33.33 -99.00  90.00   37
  9  \w     56.00 129.00   1.00    2.00    --   33.33-178.00 150.00   73
 10  \w     28.00 114.00   1.00   20.00    --   97.51-111.00 -30.00   86
 11  \w      6.00  82.00   1.00   20.00    --   97.51 -15.00 150.00   76
 12  \w    117.00 166.00   1.00   20.00    --   97.51  30.00-150.00   49
 13  \w    124.00 177.00   1.00   20.00    --   97.51 -15.00 150.00   53
 14  \w     78.00 148.00   1.00   20.00    --   97.51 178.00-150.00   70
 15  \w    111.00 150.00   1.00   20.00    --   97.51 178.00 -60.00   39
 16  \w    102.00 166.00   1.00   20.00    --   97.51 111.00 120.00   64
 17  \w     69.00 137.00   1.00   20.00    --   97.51 -61.00 -60.00   68
 18  \w     24.00  55.00   1.00   20.00    --   97.51 -61.00 -60.00   31
 19  \w     58.00 162.00   1.00   20.00    --   97.51  61.00 -90.00  104
 20  \w     65.00 138.00   1.00   20.00    --   97.51 178.00   0.00   73
 21  \w     58.00 157.00   1.00   20.00    --   97.51  45.00  90.00   99
 22  \w    129.00 168.00   1.00   20.00    --   97.51 111.00 -90.00   39
 23  \w     81.00 128.00   1.00   20.00    --   97.51 -61.00 -30.00   47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0087951000
_diffrn_orient_matrix_UB_12      0.0722640000
_diffrn_orient_matrix_UB_13      -0.0941635000
_diffrn_orient_matrix_UB_21      0.0328648000
_diffrn_orient_matrix_UB_22      -0.0657378000
_diffrn_orient_matrix_UB_23      -0.0817095000
_diffrn_orient_matrix_UB_31      -0.1074364000
_diffrn_orient_matrix_UB_32      -0.0260612000
_diffrn_orient_matrix_UB_33      -0.0549979000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.942
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14504
_diffrn_reflns_point_group_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.123
_diffrn_reflns_theta_min         4.345
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.859
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       plate
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.172
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         4147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0507P)^2^+0.4013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3850
_reflns_number_total             4147
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03311d2.cif
_cod_data_source_block           lccocpaout
_cod_depositor_comments
'Adding full bibliography for 7701168--7701171.cif.'
_cod_database_code               7701169
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     62.30
_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:
 C1(H1), C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C12(H12A,H12B), C14(H14A,H14B),
 C19(H19A,H19B), C22(H22A,H22B)
2.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C25(H25), C26(H26), C27(H27), C28(H28)
2.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C23(H23A,H23B,
 H23C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.748
_oxdiff_exptl_absorpt_empirical_full_min 0.689