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_7701443
_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            'C35 H25 Cl Fe N7 O8'
_chemical_formula_weight         762.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2018-03-24 deposited with the CCDC.    2019-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                97.572(18)
_cell_angle_beta                 112.542(17)
_cell_angle_gamma                116.508(17)
_cell_formula_units_Z            2
_cell_length_a                   13.220(19)
_cell_length_b                   14.16(2)
_cell_length_c                   14.36(2)
_cell_measurement_reflns_used    6126
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.56
_cell_measurement_theta_min      2.67
_cell_volume                     2067(5)
_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-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_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  0.0646
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            50440
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.261
_diffrn_reflns_theta_min         1.790
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Off-white
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       Block
_exptl_crystal_F_000             782
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;
The unit cell contains six disordered methanol molecule which has been treated as a diffuse contribution to the overall scatter in without 
specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.695
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         9134
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.695
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0530
_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^)+(0.2000P)^2^+0.3676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1733
_refine_ls_wR_factor_ref         0.2015
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6027
_reflns_number_total             9134
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03493e2.cif
_cod_data_source_block           rr_a_sqd
_cod_database_code               7701443
_shelx_estimated_absorpt_t_min   0.869
_shelx_estimated_absorpt_t_max   0.953
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014/6
_shelx_res_checksum              57578