Aromatic dicarboxylate incorporated new di- and tetranuclear cobalt(II) complexes: Synthetic and structural aspects, and evaluation of properties and catalytic activity
Majumder, Avishek; Dutta, Nityananda; Haldar, Shobhraj; Das, Arpan; Carrella, Luca; Bera, Manindranath; Inorganica Chimica Acta 510 (2020) 119752–; doi:10.1016/j.ica.2020.119752

data_1564405
_publ_section_title
;
 Aromatic dicarboxylate incorporated new di- and tetranuclear cobalt(II)
 complexes: Synthetic and structural aspects, and evaluation of properties
 and catalytic activity
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119752
_journal_paper_doi               10.1016/j.ica.2020.119752
_journal_volume                  510
_journal_year                    2020
_chemical_formula_moiety         '0.08(C39 H34 Co2 N4 O9), 0.4(O)'
_chemical_formula_sum            'C39 H34 Co2 N4 O14'
_chemical_formula_weight         900.54
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 91.951(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.381(3)
_cell_length_b                   12.315(3)
_cell_length_c                   26.259(7)
_cell_measurement_reflns_used    9384
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      23.115
_cell_measurement_theta_min      2.224
_cell_volume                     4001.4(17)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      125.01
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            70962
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        23.115
_diffrn_reflns_theta_max         23.115
_diffrn_reflns_theta_min         2.224
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.902
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.561
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         5587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0843P)^2^+15.3397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1483
_refine_ls_wR_factor_ref         0.1642
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4582
_reflns_number_total             5587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Co2-phthalate.cif
_cod_data_source_block           Co2-phthalate
_cod_original_cell_volume        4001.4(18)
_cod_database_code               1564405
_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 O(H) groups
2.a Ternary CH refined with riding coordinates:
 C24(H24)
2.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C32(H32A,H32B), C26(H26A,H26B), C23(H23A,H23B), C25(H25A,
 H25B), C14(H14A,H14B)
2.c Aromatic/amide H refined with riding coordinates:
 C31(H31), C28(H28), C34(H34), C37(H37), C30(H30), C36(H36), C9(H9), C35(H35),
 C8(H8), C12(H12), C11(H11), C29(H29), C5(H5), C10(H10), C17(H17), C20(H20),
 C19(H19), C18(H18), C6(H6), C7(H7)
2.d Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_shelx_res_checksum              35411
_shelx_hkl_checksum              84219
_olex2_submission_special_instructions 'No special instructions were received'