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_7701168
_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 H41 Co O10'
_chemical_formula_sum            'C34 H41 Co O10'
_chemical_formula_weight         668.60
_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
_audit_creation_date             2018-05-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-07-05 deposited with the CCDC.    2019-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.503(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7927(4)
_cell_length_b                   14.8334(3)
_cell_length_c                   13.6445(3)
_cell_measurement_reflns_used    21636
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.6080
_cell_measurement_theta_min      3.8140
_cell_volume                     3181.62(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.903
_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    -20.00  49.00   1.00   10.00    --    8.41 -99.00 -60.00   69
  2  \w    -66.00  33.00   1.00   10.00    --    8.41 -38.00-120.00   99
  3  \w    -24.00  85.00   1.00   10.00    --    8.41  77.00   0.00  109
  4  \w    -16.00  83.00   1.00   10.00    --    8.41  38.00-180.00   99
  5  \w    -16.00  83.00   1.00   10.00    --    8.41  38.00   0.00   99
  6  \w    -66.00  33.00   1.00   10.00    --    8.41 -38.00 -90.00   99
  7  \w    -16.00  83.00   1.00   10.00    --    8.41  38.00-120.00   99
  8  \w    -15.00  19.00   1.00   10.00    --    8.41-105.00 153.00   34
;
_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      0.0404202000
_diffrn_orient_matrix_UB_12      -0.0052496000
_diffrn_orient_matrix_UB_13      -0.0178771000
_diffrn_orient_matrix_UB_21      0.0101929000
_diffrn_orient_matrix_UB_22      0.0452808000
_diffrn_orient_matrix_UB_23      0.0129920000
_diffrn_orient_matrix_UB_31      0.0172519000
_diffrn_orient_matrix_UB_32      -0.0144365000
_diffrn_orient_matrix_UB_33      0.0473313000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            58452
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.589
_diffrn_reflns_theta_min         2.933
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.597
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018)
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    1.396
_exptl_crystal_description       prism
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         7338
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0679P)^2^+2.0272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1346
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5860
_reflns_number_total             7338
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03311d2.cif
_cod_data_source_block           mdl777
_cod_depositor_comments
'Adding full bibliography for 7701168--7701171.cif.'
_cod_database_code               7701168
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'c34 h41 Co1 o10'
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.860
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_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. Restrained distances
 O10-C35
 1.45 with sigma of 0.01
 O10-C33
 1.45 with sigma of 0.01
 C33-C34
 1.54 with sigma of 0.01
 C35-C36
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C33 \\sim C34: within 1.7A with sigma of 0.001 and sigma for terminal atoms of
0.002
C35 \\sim C36: within 1.7A with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(C35) = Uanis(C33)
4. Others
 Fixed Sof: C33(0.5) H33A(0.5) H33B(0.5) C34(0.5) H34A(0.5) H34B(0.5)
 H34C(0.5) C35(0.5) H35A(0.5) H35B(0.5) C36(0.5) H36A(0.5) H36B(0.5) H36C(0.5)
5.a Ternary CH refined with riding coordinates:
 C2(H2), C14(H14)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C24(H24A,H24B),
 C27(H27A,H27B), C30(H30A,H30B), C33(H33A,H33B), C35(H35A,H35B)
5.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20)
5.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C25(H25A,H25B,H25C), C28(H28A,H28B,
 H28C), C31(H31A,H31B,H31C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C)
;
_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 1.483
_oxdiff_exptl_absorpt_empirical_full_min 0.692