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_7121910
_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         'C36 H49 Co N4 O2, H2 O, 0.25(C3 H3)'
_chemical_formula_sum            'C36.75 H51.75 Co N4 O3'
_chemical_formula_weight         656.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_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                107.28(3)
_cell_angle_beta                 110.92(3)
_cell_angle_gamma                97.29(3)
_cell_formula_units_Z            2
_cell_length_a                   10.455(2)
_cell_length_b                   14.036(3)
_cell_length_c                   14.199(3)
_cell_measurement_reflns_used    21656
_cell_measurement_temperature    200
_cell_measurement_theta_max      24.997
_cell_measurement_theta_min      2.317
_cell_volume                     1793.9(9)
_computing_cell_refinement       EvalCCD
_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                 'CCD area detector'
_diffrn_detector_type            KappaCCD
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Incoatec Bruker AXS enraf noniusKappaCCD'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_collimation    'Montel optic'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21656
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.317
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.517
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.487242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.1811 before and 0.0848 after correction.
The Ratio of minimum to maximum transmission is 0.4872.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'metallic dark violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_description       needle
_exptl_crystal_F_000             702
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         6175
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0733
_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^)+(0.0786P)^2^+4.5342P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1851
_refine_ls_wR_factor_ref         0.2089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4872
_reflns_number_total             6175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04459g2.cif
_cod_data_source_block           sad
_cod_depositor_comments
'Adding full bibliography for 7121910--7121912.cif.'
_cod_original_cell_volume        1794.2(8)
_cod_database_code               7121910
_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, All O(H) groups
2. Restrained distances
 H3B-O3
 0.85 with sigma of 0.02
 H3A-H3B
 1.38 with sigma of 0.02
3. Others
 Fixed Sof: C37(0.25) H37(0.25) C38(0.25) H38(0.25) C39(0.25) H39(0.25)
4.a Free rotating group:
 O3(H3A)
4.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N4(H4), C18(H18), C11(H11), C17(H17), C5(H5), C9(H9), C16(H16),
 C3(H3), C15(H15), C37(H37), C38(H38), C39(H39)
4.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C29(H29A,H29B,H29C), C24(H24A,H24B,H24C), C32(H32A,H32B,
 H32C), C22(H22A,H22B,H22C), C33(H33A,H33B,H33C), C28(H28A,H28B,H28C), C20(H20A,
 H20B,H20C), C34(H34A,H34B,H34C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C),
 C21(H21A,H21B,H21C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              99201
_shelx_hkl_checksum              46919
_olex2_submission_special_instructions 'No special instructions were received'