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_7715274
_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         '2(C26 H33 N3 S Si Zn)'
_chemical_formula_sum            'C52 H66 N6 S2 Si2 Zn2'
_chemical_formula_weight         1026.14
_chemical_name_systematic        Zn2(triaz)2(SSiPh3)2
_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     dual
_audit_creation_date             2022-10-27
_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                 106.7230(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7677(2)
_cell_length_b                   19.2739(2)
_cell_length_c                   16.2548(2)
_cell_measurement_reflns_used    13515
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.4580
_cell_measurement_theta_min      2.5520
_cell_volume                     5331.08(11)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1947
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.975
_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   -110.00 -20.00   1.00    1.00    --  -42.17 -37.00  90.00   90
  2  \w    -86.00 -14.00   1.00    1.00    --  -42.17 125.00   0.00   72
  3  \w     19.00 113.00   1.00    1.00    --   42.17  37.00-120.00   94
  4  \w     40.00 141.00   1.00    5.00    --  112.00 -61.00 120.00  101
  5  \w     88.00 178.00   1.00    5.00    --  112.00  45.00-150.00   90
  6  \w    108.00 178.00   1.00    5.00    --  112.00 111.00 150.00   70
  7  \w    104.00 176.00   1.00    5.00    --  112.00 111.00  90.00   72
  8  \w    103.00 178.00   1.00    5.00    --  112.00  77.00-120.00   75
  9  \w     44.00 104.00   1.00    5.00    --  112.00 -94.00  60.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0076088000
_diffrn_orient_matrix_UB_12      -0.0681947000
_diffrn_orient_matrix_UB_13      -0.0512872000
_diffrn_orient_matrix_UB_21      0.0900008000
_diffrn_orient_matrix_UB_22      -0.0088255000
_diffrn_orient_matrix_UB_23      0.0302450000
_diffrn_orient_matrix_UB_31      -0.0067416000
_diffrn_orient_matrix_UB_32      -0.0407777000
_diffrn_orient_matrix_UB_33      0.0789789000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23238
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.790
_diffrn_reflns_theta_min         2.597
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.567
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.484
_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    1.279
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.131
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         10967
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0403P)^2^+0.6266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9390
_reflns_number_total             10967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00084f2.cif
_cod_data_source_block           batch3_c4_r1
_cod_depositor_comments
'Adding full bibliography for 7715272--7715274.cif.'
_cod_database_code               7715274
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C26 H33 N3 Zn1 S1 Si1'
_chemical_oxdiff_usercomment     Zn(triaz)2+Thiol
_reflns_odcompleteness_completeness 98.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C34A) \\sim Ueq, Uanis(C34B) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C34A) = Uanis(C34B)
3. Others
 Fixed Sof: C32A(0.85) H32A(0.85) H32B(0.85) H32C(0.85) C33A(0.85) H33A(0.85)
 H33B(0.85) H33C(0.85) C34A(0.85) H34A(0.85) H34B(0.85) H34C(0.85) C33B(0.15)
 H33D(0.15) H33E(0.15) H33F(0.15) C32B(0.15) H32D(0.15) H32E(0.15) H32F(0.15)
 C34B(0.15) H34D(0.15) H34E(0.15) H34F(0.15)
4.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C22(H22), C20(H20), C14(H14), C46(H46), C23(H23),
 C40(H40), C16(H16), C42(H42), C13(H13), C26(H26), C12(H12), C24(H24), C48(H48),
  C39(H39), C45(H45), C25(H25), C52(H52), C19(H19), C17(H17), C18(H18),
 C50(H50), C44(H44), C49(H49), C38(H38), C36(H36), C51(H51), C43(H43), C37(H37)
4.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C2(H2A,H2B,H2C),
 C3(H3A,H3B,H3C), C32A(H32A,H32B,H32C), C28(H28A,H28B,H28C), C8(H8A,H8B,H8C),
 C4(H4A,H4B,H4C), C33A(H33A,H33B,H33C), C34A(H34A,H34B,H34C), C7(H7A,H7B,H7C),
 C33B(H33D,H33E,H33F), C32B(H32D,H32E,H32F), C34B(H34D,H34E,H34F)
;
_shelx_res_checksum              39011
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.280
_oxdiff_exptl_absorpt_empirical_full_min 0.783