Structures and spin states of crystalline [Fe(NCS)2L2] and [FeL3]2+complexes (L = an annelated 1,10-phenanthroline derivative)
Kulmaczewski, Rafal; Halcrow, Malcolm A.; CrystEngComm 18 (2016) 2570–; doi:10.1039/C6CE00163G

data_7224622
_publ_section_title
;
 Structures and spin states of crystalline [Fe(NCS)2L2] and
 [FeL3]2+complexes (L = an annelated 1,10-phenanthroline derivative)
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2570
_journal_paper_doi               10.1039/C6CE00163G
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C66 H36 Fe N12, 2(B F4), H2 O, 3(C H4 O)'
_chemical_formula_sum            'C69 H50 B2 F8 Fe N12 O4'
_chemical_formula_weight         1340.68
_chemical_name_systematic
'Tris[dipyrido[3,2-a:23-c]benzo[i]phenazine]iron(II) di-tetrafluoroborate hydrate tris-methanol solvate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-10-12 deposited with the CCDC.
2016-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                95.037(2)
_cell_angle_beta                 98.452(2)
_cell_angle_gamma                93.612(2)
_cell_formula_units_Z            4
_cell_length_a                   9.7973(2)
_cell_length_b                   23.8139(8)
_cell_length_c                   27.5891(6)
_cell_measurement_reflns_used    11572
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      72.86
_cell_measurement_theta_min      3.57
_cell_volume                     6323.5(3)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.3095
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0694
_diffrn_reflns_av_sigmaI/netI    0.0764
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            56368
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         74.00
_diffrn_reflns_theta_min         3.25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.631
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2752
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1700
_refine_ls_number_reflns         23938
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0851
_refine_ls_shift/su_max          0.076
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1651P)^2^+0.9069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2313
_refine_ls_wR_factor_ref         0.2698
_reflns_number_gt                15545
_reflns_number_total             23938
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce00163g2.cif
_cod_data_source_block           rk119f
_cod_depositor_comments
'Adding full bibliography for 7224614--7224625.cif.'
_cod_database_code               7224622