A first exploration of isostructurality in transition metal nitroprussides: X-ray analysis, magnetic properties and DFT calculations
Pérez, Hiram; Di Santo, Alejandro; Piro, Oscar E.; Echeverría, Gustavo A.; Cano, A.; González, M.; Rodríguez-Hernández, J.; Ben Altabef, A.; Frontera, Antonio; Gil, Diego M.; CrystEngComm 23 (2021) 1158–1171; doi:10.1039/D0CE01596B

data_7241903
_publ_section_title
;
 A first exploration of isostructurality in transition metal
 nitroprussides: X-ray analysis, magnetic properties and DFT calculations
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              1158
_journal_page_last               1171
_journal_paper_doi               10.1039/D0CE01596B
_journal_volume                  23
_journal_year                    2021
_chemical_formula_sum            'C21 H24 Cu Fe N14 O'
_chemical_formula_weight         607.93
_chemical_name_systematic
catena-[bis(u-cyano)-cyano-tetrakis(1-methylimidazole)-nitrosyl-iron-copper]
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-10-03 deposited with the CCDC.	2020-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                73.752(4)
_cell_angle_beta                 80.350(4)
_cell_angle_gamma                84.476(4)
_cell_formula_units_Z            2
_cell_length_a                   9.1670(5)
_cell_length_b                   10.2296(5)
_cell_length_c                   15.6179(8)
_cell_measurement_reflns_used    3119
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      26.5470
_cell_measurement_theta_min      3.3980
_cell_volume                     1384.29(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      297(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0604
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11398
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         2.965
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.334
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       plate
_exptl_crystal_F_000             622
_exptl_crystal_recrystallization_method
'Crystals obtained from a DMF solution of the reactants by very slow evaporation of the solvent.'
_exptl_crystal_size_max          0.338
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         5585
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+0.3851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4212
_reflns_number_total             5585
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01596b2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7241902--7241906.cif.'
_cod_database_code               7241903
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.661
_shelx_estimated_absorpt_t_max   0.927
_oxdiff_exptl_absorpt_empirical_full_min 0.890
_oxdiff_exptl_absorpt_empirical_full_max 1.212
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              53791