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_7231038
_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         'C60 H31 N12 F9 Co, C4 H12 O2, H4 O2'
_chemical_formula_sum            'C64 H47 Co F9 N12 O4'
_chemical_formula_weight         1278.07
_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_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 100.471(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.1082(8)
_cell_length_b                   15.7956(5)
_cell_length_c                   20.1176(8)
_cell_measurement_reflns_used    4395
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      70.6850
_cell_measurement_theta_min      2.9880
_cell_volume                     5658.4(4)
_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 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23812
_diffrn_reflns_theta_full        73.58
_diffrn_reflns_theta_max         73.58
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    3.178
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89025
_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            orange
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2620
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_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 801 A3 containing about 240 electrons which corresponds to approximately 2 ethanol 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         0.804
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     723
_refine_ls_number_reflns         11125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1110
_refine_ls_R_factor_gt           0.0772
_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^)+(0.1497P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2246
_refine_ls_wR_factor_ref         0.2542
_reflns_number_gt                6683
_reflns_number_total             11125
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8ce00561c2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7231033--7231038.cif.'
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7231038
_oxdiff_exptl_absorpt_empirical_full_min 0.825
_oxdiff_exptl_absorpt_empirical_full_max 1.151
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;