Late First-Row Transition-Metal Complexes Containing a 2-Pyridylmethyl Pendant-Armed 15-Membered Macrocyclic Ligand. Field-Induced Slow Magnetic Relaxation in a Seven-Coordinate Cobalt(II) Compound.
Antal, Peter; Drahoš, Bohuslav; Herchel, Radovan; Trávníček, Zdeněk; Inorganic chemistry 55 (2016) 5957–5972; doi:10.1021/acs.inorgchem.6b00415

data_4347641
_publ_section_title
;
 Late First-Row Transition-Metal Complexes Containing a 2-Pyridylmethyl
 Pendant-Armed 15-Membered Macrocyclic Ligand. Field-Induced Slow Magnetic
 Relaxation in a Seven-Coordinate Cobalt(II) Compound.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5957
_journal_page_last               5972
_journal_paper_doi               10.1021/acs.inorgchem.6b00415
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C25 H31 Cl2 Fe N5 O10'
_chemical_formula_weight         688.30
_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   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 113.2370(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3758(9)
_cell_length_b                   9.1185(4)
_cell_length_c                   18.8090(8)
_cell_measurement_reflns_used    9105
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.4
_cell_volume                     2896.0(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0416
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            179792
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.591
_diffrn_reflns_theta_min         2.228
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Bruker (2015). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       prism
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_exptl_transmission_factor_max   0.949
_exptl_transmission_factor_min   0.878
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.570(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         13356
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0321P)^2^+1.6512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0681
_reflns_Friedel_coverage         0.882
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                12613
_reflns_number_total             13356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            deposit_Fe.cif
_cod_data_source_block           p
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4347641
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.861
_shelx_estimated_absorpt_t_max   0.941
_shelx_res_checksum              68917
_shelx_hkl_checksum              57171