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_4346742
_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         'C38 H27 Cl Fe N8 O2, 2(Cl O4), C3 H6 O'
_chemical_formula_sum            'C41 H33 Cl3 Fe N8 O11'
_chemical_formula_weight         975.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 103.120(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.471(6)
_cell_length_b                   22.725(18)
_cell_length_c                   10.833(8)
_cell_measurement_reflns_used    1115
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.36
_cell_measurement_theta_min      2.62
_cell_volume                     2031(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    'SHELXS (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX II QUAZAR'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_source         'multilayer monochromator ImuS'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_unetI/netI     0.1158
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6487
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        19.400
_diffrn_reflns_theta_max         19.389
_diffrn_reflns_theta_min         2.469
_exptl_absorpt_coefficient_mu    0.643
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 1021 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.08(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         3427
_refine_ls_number_restraints     425
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0090P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0835
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                2673
_reflns_number_total             3427
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02058_si_001.cif
_cod_data_source_block           CB6
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4346742
_shelx_estimated_absorpt_t_min   0.910
_shelx_estimated_absorpt_t_max   0.975
_shelxl_version_number           2014-3
_shelx_res_checksum              89322
_shelx_hkl_checksum              3678