Cobalt complexes of pyrrolecarboxamide ligands as catalysts in nitro reduction reactions: influence of electronic substituents on catalysis and mechanistic insights
Yadav, Sunil; Kumar, Sushil; Gupta, Rajeev; Inorganic Chemistry Frontiers 4 (2017) 324–; doi:10.1039/C6QI00389C

data_4349560
_publ_section_title
;
 Cobalt complexes of pyrrolecarboxamide ligands as catalysts in nitro
 reduction reactions: influence of electronic substituents on catalysis
 and mechanistic insights
;
_journal_issue                   2
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              324
_journal_paper_doi               10.1039/C6QI00389C
_journal_volume                  4
_journal_year                    2017
_chemical_formula_moiety         'C16 H8 Cl2 Co N4 O2, C8 H20 N'
_chemical_formula_sum            'C24 H28 Cl2 Co N5 O2'
_chemical_formula_weight         548.34
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-01-04 deposited with the CCDC.
2016-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      3.26
_cell_volume                     2410.6(4)
_computing_cell_refinement       'CrysAlisPro, Oxford Diffraction Ltd.,'
_computing_data_collection       'CrysAlisPro, Oxford Diffraction Ltd.,'
_computing_data_reduction        'CrysAlisPro, Oxford Diffraction Ltd.,'
_computing_molecular_graphics    'SHELXTL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  SHELXTL-2014/7
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0756
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9844
_diffrn_reflns_point_group_measured_fraction_full 0.984
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_diffrn_reflns_theta_full        24.994
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_min         3.265
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.966
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_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       cube
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_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.190
_refine_diff_density_max         1.540
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details
;
 Flack x determined using 1407 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0835
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0669P)^2^+17.2177P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2028
_refine_ls_wR_factor_ref         0.2060
_reflns_Friedel_coverage         0.751
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                3884
_reflns_number_total             4184
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6qi00389c2.cif
_cod_data_source_block           shelx
_cod_database_code               4349560
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.808
_shelx_estimated_absorpt_t_max   0.838
_exptl_absorpt_special_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_shelx_res_checksum              19118
_shelx_hkl_checksum              40692