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_7063342
_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            'C8 H6 N8 O2 Rb2 W'
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_audit_update_record
;
2024-01-26 deposited with the CCDC.	2024-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_length_b                   14.3462(3)
_cell_length_c                   12.8770(2)
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_cell_volume                     1579.03(6)
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_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
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_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.49(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
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_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
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_diffrn_reflns_point_group_measured_fraction_full 0.996
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_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
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_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.101a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.528
_exptl_crystal_description       plate
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.223
_refine_diff_density_min         -1.991
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_refine_ls_extinction_coef       0.00340(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4682
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0233
_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^)+(0.0136P)^2^+3.7309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0476
_refine_ls_wR_factor_ref         0.0491
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4026
_reflns_number_total             4682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02448f2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7063341--7063343.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7063342
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.174
_shelx_estimated_absorpt_t_max   0.346
_shelx_res_checksum              55861
_shelx_hkl_checksum              36589