Synthesis, characterisation and reactivity of a zinc triazenide for potential use in vapour deposition.
Samii, Rouzbeh; Barkas, Essi; Zanders, David; Fransson, Anton; Lahtinen, Manu; Kessler, Vadim; Tuononen, Heikki M.; Moilanen, Jani O.; O'Brien, Nathan J; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5911–5916; doi:10.1039/d4dt00084f

data_7715272
_publ_section_title
;
 Synthesis, characterisation and reactivity of a zinc triazenide for
 potential use in vapour deposition.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5911
_journal_page_last               5916
_journal_paper_doi               10.1039/d4dt00084f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C32 H72 N12 Zn2'
_chemical_formula_sum            'C32 H72 N12 Zn2'
_chemical_formula_weight         755.75
_chemical_name_systematic        Zn2(triaz)4
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-10-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-01-10 deposited with the CCDC.	2024-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.5640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.46540(10)
_cell_length_b                   11.07540(10)
_cell_length_c                   18.2679(2)
_cell_measurement_reflns_used    14014
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.3100
_cell_measurement_theta_min      4.2730
_cell_volume                     2074.42(4)
_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_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120.15
_diffrn_detector_area_resol_mean 5.1947
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -122.00  -1.00   1.00    2.00    --  -42.17 -19.00  30.00  121
  2  \w    -83.00  38.00   1.00    2.00    --  -42.17  19.00-150.00  121
  3  \w      6.00  83.00   1.00    2.00    --   42.17 -99.00 -60.00   77
  4  \w     27.00  98.00   1.00    2.00    --   42.17-125.00-150.00   71
  5  \w     27.00  98.00   1.00    2.00    --   42.17-125.00  90.00   71
  6  \w     36.00 109.00   1.00   12.50    --  112.00-111.00-120.00   73
  7  \w     40.00 141.00   1.00   12.50    --  112.00 -61.00-150.00  101
  8  \w     83.00 178.00   1.00   12.50    --  112.00  61.00  30.00   95
  9  \w     36.00 109.00   1.00   12.50    --  112.00-111.00  30.00   73
 10  \w     83.00 178.00   1.00   12.50    --  112.00  61.00   0.00   95
 11  \w    104.00 178.00   1.00   12.50    --  112.00 111.00-120.00   74
 12  \w     83.00 178.00   1.00   12.50    --  112.00  61.00  60.00   95
 13  \w     83.00 178.00   1.00   12.50    --  112.00  61.00 -60.00   95
 14  \w     36.00 109.00   1.00   12.50    --  112.00-111.00 -30.00   73
 15  \w     36.00 109.00   1.00   12.50    --  112.00-111.00 120.00   73
 16  \w    103.00 178.00   1.00   12.50    --  112.00  77.00-150.00   75
 17  \w     61.00 146.00   1.00   12.50    --  112.00 178.00 -90.00   85
 18  \w   -114.00 -14.00   1.00    2.00    --  -42.17 -57.00-150.00  100
 19  \w   -114.00 -14.00   1.00    2.00    --  -42.17 -57.00 -30.00  100
 20  \w   -114.00 -14.00   1.00    2.00    --  -42.17 -57.00-120.00  100
 21  \w     14.00 114.00   1.00    2.00    --   42.17  57.00-180.00  100
 22  \w     86.00 178.00   1.00   12.50    --  112.00  45.00 120.00   92
 23  \w     84.00 178.00   1.00   12.50    --  112.00  30.00-180.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24531
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.607
_diffrn_reflns_theta_min         4.312
_exptl_absorpt_coefficient_mu    1.695
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         4318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0331P)^2^+1.1148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0737
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3854
_reflns_number_total             4318
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00084f2.cif
_cod_data_source_block           batch4-c1-2-r1
_cod_depositor_comments
'Adding full bibliography for 7715272--7715274.cif.'
_cod_database_code               7715272
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.862
_shelx_estimated_absorpt_t_min   0.778
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C11(H11A,H11B,H11C), C16(H16A,H16B,
 H16C), C3(H3A,H3B,H3C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C), C8(H8A,H8B,
 H8C), C7(H7A,H7B,H7C), C4(H4A,H4B,H4C), C2(H2A,H2B,H2C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              71885
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;