Dioxygen Reactivity of Iron(II)-Gentisate/1,4-Dihydroxy-2-naphthoate Complexes of N4 Ligands: Oxidative Coupling of 1,4-Dihydroxy-2-naphthoate
Paine, Tapan Kanti; Rahaman, Rubina; Munshi, Sandip; Banerjee, Sridhar; Chakraborty, Biswarup; Bhunia, Sarmistha; Dalton Transactions  (2019) –; doi:10.1039/C9DT03493E

data_7701439
_publ_section_title
;
 Dioxygen Reactivity of Iron(II)-Gentisate/1,4-Dihydroxy-2-naphthoate
 Complexes of N4 Ligands: Oxidative Coupling of 1,4-Dihydroxy-2-naphthoate
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03493E
_journal_year                    2019
_chemical_formula_sum            'C57 H61 B Cl2 Fe N4 O5'
_chemical_formula_weight         1019.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-03-24 deposited with the CCDC.    2019-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.576(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.700(3)
_cell_length_b                   9.7342(14)
_cell_length_c                   26.459(4)
_cell_measurement_reflns_used    7806
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.03
_cell_measurement_theta_min      2.24
_cell_volume                     5182.5(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_unetI/netI     0.0663
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            34388
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        22.976
_diffrn_reflns_theta_max         22.976
_diffrn_reflns_theta_min         1.129
_exptl_absorpt_coefficient_mu    0.447
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       Block
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.306
_refine_diff_density_min         -1.120
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         7096
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1183
_refine_ls_R_factor_gt           0.0825
_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^)+(0.1334P)^2^+19.8218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2210
_refine_ls_wR_factor_ref         0.2557
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5161
_reflns_number_total             7096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03493e2.cif
_cod_data_source_block           BC228B_0m
_cod_database_code               7701439
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.878
_shelx_estimated_absorpt_t_max   0.957
_shelx_res_checksum              40719