Iron(ii) and cobalt(ii) complexes based on anionic phenanthroline-imidazolate ligands: reversible single-crystal-to-single-crystal transformations
Abhervé, Alexandre; Benmansour, Samia; Gómez-García, Carlos José; Avarvari, Narcis; CrystEngComm 20 (2018) 4141–; doi:10.1039/C8CE00561C

data_7231036
_publ_section_title
;
 Iron(ii) and cobalt(ii) complexes based on anionic
 phenanthroline-imidazolate ligands: reversible
 single-crystal-to-single-crystal transformations
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              4141
_journal_paper_doi               10.1039/C8CE00561C
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'Fe C60 H30 F9 N12, C8 H24 O4, H14 O7'
_chemical_formula_sum            'C68 H68 F9 Fe N12 O11'
_chemical_formula_weight         1456.19
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-04-08 deposited with the CCDC.
2018-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.7212(4)
_cell_length_b                   18.6855(6)
_cell_length_c                   20.2478(4)
_cell_measurement_reflns_used    8173
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.8810
_cell_measurement_theta_min      3.4230
_cell_volume                     6704.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 5.1990
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26628
_diffrn_reflns_theta_full        73.41
_diffrn_reflns_theta_max         73.41
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    2.629
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85284
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3020
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
The unit cell contains disordered ethanol and water molecules which were not modelled but the corresponding scattering contribution were taken into account using SQUEEZE/PLATON procedure. The unit cell contains a void of 2055 A3 containing about 593 electrons which corresponds to approximately 3 ethanol molecules and 7 water molecules per formula unit. The solvent composition was included in the calculation of the empirical formula, formula weight, density, linear absorption coefficient and F(000).
;
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.024(4)
_refine_ls_extinction_coef       0.00008(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         12452
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0618
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1274P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1705
_refine_ls_wR_factor_ref         0.1839
_reflns_number_gt                10164
_reflns_number_total             12452
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8ce00561c2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7231033--7231038.cif.'
_cod_database_code               7231036
_oxdiff_exptl_absorpt_empirical_full_min 0.789
_oxdiff_exptl_absorpt_empirical_full_max 1.152
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;