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_7231033
_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         'H9 O4, C57 H33 N12 Fe, C8 H20 O2, H2 O'
_chemical_formula_sum            'C65 H64 Fe N12 O7'
_chemical_formula_weight         1181.13
_space_group_IT_number           144
_space_group_name_Hall           'P 31'
_space_group_name_H-M_alt        'P 31'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31'
_symmetry_space_group_name_H-M   'P 31'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   16.9172(2)
_cell_length_b                   16.9172(2)
_cell_length_c                   17.9975(3)
_cell_measurement_reflns_used    11806
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.4160
_cell_measurement_theta_min      2.9570
_cell_volume                     4460.67(11)
_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_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 5.1990
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33065
_diffrn_reflns_theta_full        73.55
_diffrn_reflns_theta_max         73.55
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    2.562
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72629
_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    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1860
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
The unit cell contains disordered solvent 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 344 A3 containing about 28 electrons which corresponds to approximately 1 water molecule 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         0.439
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         10971
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+0.3008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1048
_reflns_number_gt                10111
_reflns_number_total             10971
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8ce00561c2.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 7231033--7231038.cif.'
_cod_original_cell_volume        4460.66(11)
_cod_original_sg_symbol_H-M      P31
_cod_database_code               7231033
_oxdiff_exptl_absorpt_empirical_full_min 0.749
_oxdiff_exptl_absorpt_empirical_full_max 1.216
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;