Pyridinediimine Iron Complexes with Pendant Redox-Inactive Metals Located in the Secondary Coordination Sphere.
Delgado, Mayra; Ziegler, Joshua M.; Seda, Takele; Zakharov, Lev N.; Gilbertson, John D.; Inorganic chemistry 55 (2016) 555–557; doi:10.1021/acs.inorgchem.5b02544

data_4344622
_publ_section_title
;
 Pyridinediimine Iron Complexes with Pendant Redox-Inactive Metals Located
 in the Secondary Coordination Sphere.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              555
_journal_page_last               557
_journal_paper_doi               10.1021/acs.inorgchem.5b02544
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C34 H47 Fe N3 O7'
_chemical_formula_weight         665.59
_chemical_name_systematic
;
 ?
;
_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-2013
_cell_angle_alpha                114.394(3)
_cell_angle_beta                 103.191(4)
_cell_angle_gamma                90.234(4)
_cell_formula_units_Z            2
_cell_length_a                   8.6642(17)
_cell_length_b                   13.636(3)
_cell_length_c                   16.314(3)
_cell_measurement_reflns_used    4481
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.45
_cell_measurement_theta_min      2.48
_cell_volume                     1698.5(6)
_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-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 1.000
_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  0.0992
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_laue_measured_fraction_full 0.970
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33984
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.416
_diffrn_source                   'sealed tube and triumph'
_exptl_absorpt_coefficient_mu    0.494
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       plate
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.147
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0575
_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^)+(0.0674P)^2^+2.4846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1331
_refine_ls_wR_factor_ref         0.1565
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4150
_reflns_number_total             5980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02544_si_002.cif
_cod_data_source_block           mo_g173_0m
_cod_original_cell_volume        1698.6(6)
_cod_database_code               4344622
_shelx_estimated_absorpt_t_min   0.912
_shelx_estimated_absorpt_t_max   0.976
_shelxl_version_number           2013-4
_shelx_res_checksum              7375
_shelx_hkl_checksum              62917