Six- and seven-coordinate Fe(ii) and Zn(ii) compounds ligated by unsymmetric xanthene-based ligands: characterization and magnetic properties
Haas, Ruth M.; Arshad, Muhammad; Anthony, James; Altmann, Philipp J.; Pöthig, Alexander; Köhler, Frank H.; Hess, Corinna R.; Inorganic Chemistry Frontiers 3 (2016) 616–; doi:10.1039/C5QI00298B

data_4349101
_publ_section_title
;
 Six- and seven-coordinate Fe(ii) and Zn(ii) compounds ligated by
 unsymmetric xanthene-based ligands: characterization and magnetic
 properties
;
_journal_issue                   5
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              616
_journal_paper_doi               10.1039/C5QI00298B
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety         'C41 H45 Fe N5 O, 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C43 H48 F12 Fe N6 O P2'
_chemical_formula_weight         1010.66
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2015-12-16 deposited with the CCDC.
2016-02-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.641(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6546(17)
_cell_length_b                   14.2997(14)
_cell_length_c                   18.8804(19)
_cell_measurement_reflns_used    9101
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.4295
_cell_measurement_theta_min      2.7926
_cell_volume                     4761.4(8)
_computing_cell_refinement       'SAINT (Bruker, 2012)'
_computing_data_collection       'APEX II Control Software (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2012)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2014)'
_computing_structure_refinement
'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  'MONTEL optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'rotating anode FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0156
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            203262
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_crystal_colour            'intense red'
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.323
_exptl_crystal_size_mid          0.284
_exptl_crystal_size_min          0.267
_refine_diff_density_max         0.807
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         13923
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'W=1/[\S^2^(FO^2^)+(0.0540P)^2^+3.7558P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1105
_reflns_number_gt                12389
_reflns_number_total             13923
_reflns_threshold_expression     i>2\s(i)
_cod_data_source_file            c5qi00298b2.cif
_cod_data_source_block           haaru6_0m
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4349101
_shelx_res_checksum              79446
_shelx_hkl_checksum              52132