X-ray crystal structures of K+ and Rb+ salts of [W(CN)6(bpy)]2− ion. The unusual cation‒anion interactions and structure changes going from Li+ to Cs+ salts
Hodorowicz, Maciej; Jurowska, Anna; Szklarzewicz, Janusz; CrystEngComm 23 (2021) 1207–1217; doi:10.1039/D0CE01674H

data_7241966
_publ_section_title
;
 X-ray crystal structures of K+ and Rb+ salts of [W(CN)6(bpy)]2&#x2212;
 ion. The unusual cation--anion interactions and structure changes going
 from Li+ to Cs+ salts
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              1207
_journal_page_last               1217
_journal_paper_doi               10.1039/D0CE01674H
_journal_volume                  23
_journal_year                    2021
_chemical_formula_sum            'C32 H16 N16 O7 Rb4 W2'
_chemical_formula_weight         1446.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-11-07 deposited with the CCDC.	2020-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.2200(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.6594(3)
_cell_length_b                   9.23330(10)
_cell_length_c                   17.6019(2)
_cell_measurement_reflns_used    73088
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      32.0270
_cell_measurement_theta_min      2.2590
_cell_volume                     4325.94(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1189
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            157577
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.871
_diffrn_reflns_theta_min         2.295
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.849
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.221
_exptl_crystal_description       plate
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.200
_refine_diff_density_min         -1.777
_refine_diff_density_rms         0.291
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         13504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0417P)^2^+27.1841P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11256
_reflns_number_total             13504
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01674h1.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7241966--7241967.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7241966
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.243
_shelx_estimated_absorpt_t_max   0.639
_shelx_res_checksum              16525