Homoleptic versus Heteroleptic Formation of Mononuclear Fe(II) Complexes with Tris-Imine Ligands.
Barrios, Leoní A; Bartual-Murgui, Carlos; Peyrecave-Lleixà, Eugènia; Le Guennic, Boris; Teat, Simon J.; Roubeau, Olivier; Aromí, Guillem; Inorganic chemistry 55 (2016) 4110–4116; doi:10.1021/acs.inorgchem.5b02058

data_4346745
_publ_section_title
;
 Homoleptic versus Heteroleptic Formation of Mononuclear Fe(II) Complexes
 with Tris-Imine Ligands.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4110
_journal_page_last               4116
_journal_paper_doi               10.1021/acs.inorgchem.5b02058
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C42 H30 Fe N10 O2, 2(Cl O4), 3(C3 H6 O)'
_chemical_formula_sum            'C51 H48 Cl2 Fe N10 O13'
_chemical_formula_weight         1135.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                77.619(5)
_cell_angle_beta                 67.345(7)
_cell_angle_gamma                67.933(9)
_cell_formula_units_Z            2
_cell_length_a                   13.606(3)
_cell_length_b                   13.738(4)
_cell_length_c                   16.260(5)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.62
_cell_measurement_theta_min      2.94
_cell_volume                     2590.7(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44494
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        33.050
_diffrn_reflns_theta_max         33.072
_diffrn_reflns_theta_min         2.105
_exptl_absorpt_coefficient_mu    0.588
_exptl_absorpt_correction_T_max  0.747
_exptl_absorpt_correction_T_min  0.707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 - Bruker AXS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.536
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         15137
_refine_ls_number_restraints     288
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0622P)^2^+2.4794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12684
_reflns_number_total             15137
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02058_si_010.cif
_cod_data_source_block           cb133_a
_cod_database_code               4346745
_shelx_estimated_absorpt_t_min   0.944
_shelx_estimated_absorpt_t_max   0.954
_shelxl_version_number           2014-3
_shelx_res_checksum              48519
_shelx_hkl_checksum              9105