Crystal structure and infrared and Raman spectra of K3[Cr(CN)5NO].2H2O, a member of an iconic family of complexes in coordination chemistry
Piro, Oscar E.; Echeverría, Gustavo A.; Navaza, Alda; Güida, Jorge A.; Inorganica Chimica Acta 511 (2020) 119831–; doi:10.1016/j.ica.2020.119831

data_1564183
_publ_section_title
;
 Crystal structure and infrared and Raman spectra of K3[Cr(CN)5NO].2H2O, a
 member of an iconic family of complexes in coordination chemistry
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119831
_journal_paper_doi               10.1016/j.ica.2020.119831
_journal_volume                  511
_journal_year                    2020
_chemical_formula_sum            'C5 H4 Cr K3 N6 O3'
_chemical_formula_weight         365.44
_chemical_name_systematic
'potassium pentacyanonitrosylchromate(I) dihydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 118.005(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8379(6)
_cell_length_b                   7.1589(2)
_cell_length_c                   11.5293(4)
_cell_measurement_reflns_used    2592
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      27.9330
_cell_measurement_theta_min      3.9900
_cell_volume                     1299.89(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.873
_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  0.0214
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.873
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4981
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.873
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.801
_diffrn_reflns_theta_min         3.126
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.848
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89143
_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            green
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_description       fragment
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.113
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.26(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         2380
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0332P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0671
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.873
_reflns_number_gt                2251
_reflns_number_total             2380
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-521-119831.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               1564183
_shelx_estimated_absorpt_t_min   0.723
_shelx_estimated_absorpt_t_max   0.818
_oxdiff_exptl_absorpt_empirical_full_min 0.876
_oxdiff_exptl_absorpt_empirical_full_max 1.162
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              74098
_shelx_hkl_checksum              34185