Anion–cation interactions in a series of salts with substituted Hphen, Hbpy and H2bpy cations and [W(CN)8]4− anion: polymer with “super-short” N–H⋯N hydrogen bridges containing exclusively anions and H+
Jurowska, Anna; Hodorowicz, Maciej; Kruczała, Krzysztof; Szklarzewicz, Janusz; Dalton Transactions  (2021) –; doi:10.1039/D1DT03224K

data_7708956
_publ_section_title
;
 Anion--cation interactions in a series of salts with substituted Hphen,
 Hbpy and H2bpy cations and [W(CN)8]4&#x2212; anion: polymer with
 &#x201C;super-short&#x201D; N--H&#x22EF;N hydrogen bridges containing
 exclusively anions and H+
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03224K
_journal_year                    2021
_chemical_formula_sum            'C44 H45 N14 O4 W'
_chemical_formula_weight         1017.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2021-05-19 deposited with the CCDC.	2021-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.0470(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.49300(10)
_cell_length_b                   12.54760(10)
_cell_length_c                   21.7724(2)
_cell_measurement_reflns_used    36772
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      30.3660
_cell_measurement_theta_min      2.8340
_cell_volume                     4517.30(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      130.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_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  0.0345
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            74967
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.556
_diffrn_reflns_theta_min         2.545
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.616
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       prism
_exptl_crystal_F_000             2052
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.676
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         13157
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0203P)^2^+9.0413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11384
_reflns_number_total             13157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03224k2.cif
_cod_data_source_block           shelx_CCDC1
_cod_original_cell_volume        4517.29(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7708956
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.780
_shelx_estimated_absorpt_t_max   0.780
_shelx_res_checksum              61314
_shelx_hkl_checksum              73901