Electrochemical, spectroscopic, magnetic and structural studies of complexes bearing ferrocenyl ligands of N-(3-hydroxypicolinoyl)picolinamide
Gasser, Gilles; Mari, Cristina; Burkart, Michelle; Green, Stephen J.; Ribas, Joan; Stoeckli-Evans, Helen; Tucker, James H. R.; New Journal of Chemistry 36 (2012) 1819–; doi:10.1039/c2nj40177k

data_7052923
_publ_section_title
;
 Electrochemical, spectroscopic, magnetic and structural studies of
 complexes bearing ferrocenyl ligands of
 N-(3-hydroxypicolinoyl)picolinamide
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1819
_journal_paper_doi               10.1039/c2nj40177k
_journal_volume                  36
_journal_year                    2012
_chemical_formula_moiety         'C36 H24 Fe N6 O8, 2(C H Cl3)'
_chemical_formula_sum            'C38 H26 Cl6 Fe N6 O8'
_chemical_formula_weight         963.20
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2011-06-03 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.029(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.391(5)
_cell_length_b                   18.117(5)
_cell_length_c                   13.078(5)
_cell_measurement_reflns_used    19933
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.54
_cell_measurement_theta_min      1.50
_cell_volume                     3883(2)
_computing_cell_refinement       X-Area
_computing_data_collection       'X-Area (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED32 (Stoe & Cie, 2002)'
_computing_molecular_graphics
'PLATON (Spek, 2009) and Mercury (Macrae et al., 2006)'
_computing_publication_material
'SHELXL-97, PLATON and Publcif (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\f + \w scans'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25659
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.68
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9415
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULscanABS in PLATON (Spek, 2009)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         6912
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0961
_reflns_number_gt                5050
_reflns_number_total             6912
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2nj40177k.txt
_cod_data_source_block           H2L2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7052923