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_7701170
_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         'C34 H38 Co N O8 S, C2 H3 N'
_chemical_formula_sum            'C36 H41 Co N2 O8 S'
_chemical_formula_weight         720.70
_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             2017-02-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2018-07-05 deposited with the CCDC.    2019-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.3497(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.07112(12)
_cell_length_b                   14.17053(18)
_cell_length_c                   26.6353(4)
_cell_measurement_reflns_used    9835
_cell_measurement_temperature    293
_cell_measurement_theta_max      74.0000
_cell_measurement_theta_min      4.5330
_cell_volume                     3417.92(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9b (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    '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 1.000
_diffrn_measured_fraction_theta_max 0.985
_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   -114.00 -29.00   1.00    8.00    --  -41.07 -38.00-150.00   85
  2  \w    -63.00 -28.00   1.00    8.00    --  -41.07  57.00 -90.00   35
  3  \w   -113.00 -17.00   1.00    8.00    --  -41.07 -57.00 120.00   96
  4  \w    -53.00  23.00   1.00    8.00    --  -41.07  38.00-180.00   76
  5  \w   -115.00 -28.00   1.00    8.00    --  -41.07 -38.00   0.00   87
  6  \w     -9.00  25.00   1.00    8.00    --   41.07 -38.00 -60.00   34
  7  \w     96.00 129.00   1.00   30.00    --  107.87 125.00  60.00   33
  8  \w     83.00 178.00   1.00   30.00    --  107.87  45.00 -60.00   95
  9  \w     42.00  91.00   1.00   30.00    --  107.87-125.00-120.00   49
 10  \w     58.00 103.00   1.00   30.00    --  107.87 -94.00 -90.00   45
 11  \w     83.00 176.00   1.00   30.00    --  107.87  45.00   0.00   93
 12  \w     80.00 122.00   1.00   30.00    --  107.87-125.00-150.00   42
 13  \w     85.00 110.00   1.00   30.00    --  107.87-125.00 120.00   25
 14  \w    104.00 172.00   1.00   30.00    --  107.87  61.00-120.00   68
 15  \w     40.00  69.00   1.00   30.00    --  107.87-125.00-150.00   29
 16  \w     44.00 106.00   1.00   30.00    --  107.87 -45.00-180.00   62
 17  \w     57.00 132.00   1.00   30.00    --  107.87 -61.00  30.00   75
 18  \w     26.00  53.00   1.00   30.00    --  107.87 -94.00 -30.00   27
 19  \w     81.00 107.00   1.00   30.00    --  107.87 -94.00 -30.00   26
 20  \w     42.00 135.00   1.00   30.00    --  107.87 -61.00 -60.00   93
 21  \w    153.00 178.00   1.00   30.00    --  107.87  45.00 -90.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0766303000
_diffrn_orient_matrix_UB_12      0.0967377000
_diffrn_orient_matrix_UB_13      -0.0027490000
_diffrn_orient_matrix_UB_21      0.0322305000
_diffrn_orient_matrix_UB_22      -0.0191174000
_diffrn_orient_matrix_UB_23      -0.0552299000
_diffrn_orient_matrix_UB_31      -0.1484037000
_diffrn_orient_matrix_UB_32      0.0458278000
_diffrn_orient_matrix_UB_33      -0.0172694000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            24414
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.163
_diffrn_reflns_theta_min         3.534
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.963
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9b (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    1.401
_exptl_crystal_description       prism
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         6847
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0668P)^2^+0.9790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1130
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6167
_reflns_number_total             6847
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03311d2.cif
_cod_data_source_block           mdl326
_cod_depositor_comments
'Adding full bibliography for 7701168--7701171.cif.'
_cod_database_code               7701170
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'c30 h30 Co1 n1 o8 s1'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Rigid bond restraints
 C23, C27, C26, C25, C24
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3.a Ternary CH refined with riding coordinates:
 C5(H5), C11(H11)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C14(H14A,H14B), C16(H16A,H16B), C18(H18A,H18B),
 C21(H21A,H21B)
3.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C29(H29), C30(H30),
 C32(H32), C33(H33)
3.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C19(H19A,H19B,H19C), C22(H22A,H22B,
 H22C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C)
;
_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 1.365
_oxdiff_exptl_absorpt_empirical_full_min 0.809