A highly active diradical cobalt(iii) catalyst for the cycloisomerization of alkynoic acids.
Leconte, Nicolas; du Moulinet d'Hardemare, Amaury; Philouze, Christian; Thomas, Fabrice; Chemical communications (Cambridge, England) 54 (2018) 8241–8244; doi:10.1039/c8cc04459g

data_7121912
_publ_section_title
;
 A highly active diradical cobalt(iii) catalyst for the cycloisomerization
 of alkynoic acids.
;
_journal_issue                   59
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8241
_journal_page_last               8244
_journal_paper_doi               10.1039/c8cc04459g
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C34 H46 Cl Co N4, C2 H3 N'
_chemical_formula_sum            'C36 H49 Cl Co N5'
_chemical_formula_weight         646.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-06-01
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-01 deposited with the CCDC.
2018-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.83(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.519(3)
_cell_length_b                   16.983(3)
_cell_length_c                   14.819(3)
_cell_measurement_reflns_used    38863
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.997
_cell_measurement_theta_min      2.671
_cell_volume                     3458.5(13)
_computing_cell_refinement       'Bruker Enraf Nonius kappa CCD'
_computing_data_collection       Collect
_computing_data_reduction        EvalCCD
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38863
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.997
_diffrn_reflns_theta_min         2.671
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.877920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.1059 before and 0.0359 after correction.
The Ratio of minimum to maximum transmission is 0.8779.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_description       prism
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         8257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0286P)^2^+2.2127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0918
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6573
_reflns_number_total             8257
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04459g2.cif
_cod_data_source_block           sad_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7121910--7121912.cif.'
_cod_database_code               7121912
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N4(H4), N1(H1), C11(H11), C17(H17), C18(H18), C15(H15), C16(H16), C5(H5),
 C9(H9), C3(H3)
2.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C21(H21A,H21B,H21C), C20(H20A,H20B,
 H20C), C22(H22A,H22B,H22C), C30(H30A,H30B,H30C), C25(H25A,H25B,H25C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C),
 C26(H26A,H26B,H26C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              84730
_shelx_hkl_checksum              79244
_olex2_submission_special_instructions 'No special instructions were received'