Valence directed binding mode of [2 × 2] iron grids of an unsymmetrical picolinic hydrazone based ligand
Hossain, Sayed Muktar; Lakma, Avinash; Pradhan, Rabindra Nath; Demeshko, Serhiy; Singh, Akhilesh Kumar; Dalton Transactions 46 (2017) 12612–12618; doi:10.1039/C7DT02433A

data_1546809
_publ_section_title
;
 Valence directed binding mode of [2 \\times 2] iron grids of an
 unsymmetrical picolinic hydrazone based ligand
;
_journal_issue                   37
_journal_name_full               'Dalton Transactions'
_journal_page_first              12612
_journal_page_last               12618
_journal_paper_doi               10.1039/C7DT02433A
_journal_volume                  46
_journal_year                    2017
_chemical_formula_sum            'C60 H40 Fe4 N12 O16'
_chemical_formula_weight         1408.44
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-08-16 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.0581(11)
_cell_length_b                   15.0581(11)
_cell_length_c                   12.1751(9)
_cell_measurement_reflns_used    3424
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.41
_cell_measurement_theta_min      2.15
_cell_volume                     2760.7(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1832
_diffrn_reflns_av_unetI/netI     0.1203
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            132353
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.413
_diffrn_reflns_theta_min         2.151
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.118
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_description       Block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.988
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Flack x determined using 708 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3424
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.1641
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+0.0173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1469
_reflns_Friedel_coverage         0.788
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                2021
_reflns_number_total             3424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02433a2.cif
_cod_data_source_block           1
_cod_original_cell_volume        2760.7(5)
_cod_database_code               1546809
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              75017