Synthesis of diaminoacetylene from cyanido ligands of the octacyanidotungstate complex
Szklarzewicz, Janusz; Hodorowicz, Maciej; Jurowska, Anna; New Journal of Chemistry 48 (2024) 13196–13205; doi:10.1039/D4NJ02448F

data_7063343
_publ_section_title
;
 Synthesis of diaminoacetylene from cyanido ligands of the
 octacyanidotungstate complex
;
_journal_issue                   29
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13196
_journal_page_last               13205
_journal_paper_doi               10.1039/D4NJ02448F
_journal_volume                  48
_journal_year                    2024
_chemical_formula_sum            'C16 Cs4 N16 O W2'
_chemical_formula_weight         1331.66
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_space_group_name_Hall           'P -2yc'
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_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-02-07 deposited with the CCDC.	2024-07-04 downloaded from the CCDC.
;
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_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
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_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.861
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
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_diffrn_reflns_limit_l_min       -19
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_diffrn_reflns_point_group_measured_fraction_full 0.978
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_diffrn_reflns_theta_max         30.856
_diffrn_reflns_theta_min         3.344
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.100a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.923
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
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_refine_diff_density_min         -2.067
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_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.299(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    undef
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_refine_ls_number_reflns         7379
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_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0567P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0846
_reflns_Friedel_coverage         0.795
_reflns_Friedel_fraction_full    0.958
_reflns_Friedel_fraction_max     0.687
_reflns_number_gt                7124
_reflns_number_total             7379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02448f2.cif
_cod_data_source_block           shelx_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7063341--7063343.cif.'
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               7063343
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.119
_shelx_estimated_absorpt_t_max   0.790
_shelx_res_checksum              82303
_shelx_hkl_checksum              4867