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_4346744
_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         'C30 H22 Fe N6, 2(Cl O4), H2 O'
_chemical_formula_sum            'C30 H24 Cl2 Fe N6 O9'
_chemical_formula_weight         739.30
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 91.950(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7293(4)
_cell_length_b                   8.7613(5)
_cell_length_c                   38.725(2)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.83
_cell_measurement_theta_min      2.29
_cell_volume                     2960.0(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            45305
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        33.050
_diffrn_reflns_theta_max         33.072
_diffrn_reflns_theta_min         2.295
_exptl_absorpt_coefficient_mu    0.898
_exptl_absorpt_correction_T_max  0.747
_exptl_absorpt_correction_T_min  0.645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/4
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.946
_refine_diff_density_min         -1.321
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.231
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         8630
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.231
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0785
_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^)+(0.0228P)^2^+19.2178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1769
_refine_ls_wR_factor_ref         0.1800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7493
_reflns_number_total             8630
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02058_si_005.cif
_cod_data_source_block           cb9block
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4346744
_shelx_estimated_absorpt_t_min   0.916
_shelx_estimated_absorpt_t_max   0.932
_shelxl_version_number           2014-3
_shelx_res_checksum              58272
_shelx_hkl_checksum              31961