Synthesis of a pentadentate, polypyrazine ligand and its application in cobalt-catalyzed hydrogen production
Chen, Lizhu; Khadivi, Amir; Singh, Manpreet; Jurss, Jonah W.; Inorganic Chemistry Frontiers 4 (2017) 1649–; doi:10.1039/C7QI00362E

data_4349759
_publ_section_title
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 Synthesis of a pentadentate, polypyrazine ligand and its application in
 cobalt-catalyzed hydrogen production
;
_journal_issue                   10
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1649
_journal_paper_doi               10.1039/C7QI00362E
_journal_volume                  4
_journal_year                    2017
_chemical_formula_moiety         'C32 H31 Co F6 N13 O7 S2'
_chemical_formula_sum            'C32 H31 Co F6 N13 O7 S2'
_chemical_formula_weight         946.75
_chemical_name_common            '[(PZ5Me2)Co(OH2)](OTf)2'
_chemical_name_systematic
'aqua(2,6-bis(1,1-bis(2-pyrazyl)ethyl)pyrazine)cobalt(II) trifluoromethanesulfonate'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-02-24 deposited with the CCDC.
2017-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 113.296(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9091(7)
_cell_length_b                   18.0464(9)
_cell_length_c                   16.7575(8)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.05
_cell_measurement_theta_min      3.77
_cell_volume                     3863.4(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'HELIOS multilayer mirrors'
_diffrn_radiation_source         'microfocus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30862
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         68.33
_diffrn_reflns_theta_min         3.46
_exptl_absorpt_coefficient_mu    5.343
_exptl_absorpt_correction_T_max  0.4000
_exptl_absorpt_correction_T_min  0.3604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shards
_exptl_crystal_F_000             1932
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         6876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0161P)^2^+36.6384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1820
_refine_ls_wR_factor_ref         0.1854
_reflns_number_gt                6053
_reflns_number_total             6876
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7qi00362e2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
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_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4349759