Brønsted and Lewis acid adducts of triazenes.
Landman, Iris R.; Suleymanov, Abdusalom A.; Fadaei-Tirani, Farzaneh; Scopelliti, Rosario; Chadwick, F. Mark; Severin, Kay; Dalton transactions (Cambridge, England : 2003) 49 (2020) 2317–2322; doi:10.1039/d0dt00049c

data_7703445
_publ_section_title
;
 Br\/onsted and Lewis acid adducts of triazenes.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2317
_journal_page_last               2322
_journal_paper_doi               10.1039/d0dt00049c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C28 H38 Cl2 N6 O4 Pd'
_chemical_formula_sum            'C28 H38 Cl2 N6 O4 Pd'
_chemical_formula_weight         699.94
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-08-14
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.07.31 svn.r3643 for OlexSys, GUI svn.r5859)
;
_audit_update_record
;
2019-11-20 deposited with the CCDC.	2020-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                98.576(4)
_cell_angle_beta                 106.738(4)
_cell_angle_gamma                90.520(4)
_cell_formula_units_Z            1
_cell_length_a                   8.1628(4)
_cell_length_b                   8.4628(4)
_cell_length_c                   12.1951(6)
_cell_measurement_reflns_used    4060
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      75.7560
_cell_measurement_theta_min      5.2700
_cell_volume                     796.52(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.56a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.56a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.56a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_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   -120.00 -94.00   1.00    1.00    --  -43.01 -99.00  90.00   26
  2  \w   -121.00 -94.00   1.00    1.00    --  -43.01 -99.00   0.00   27
  3  \w    -67.00  27.00   1.00    1.00    --  -43.01  37.00  30.00   94
  4  \w    -66.00  31.00   1.00    1.00    --  -43.01  37.00 120.00   97
  5  \w      7.00  32.00   1.00    1.00    --   43.01 -99.00-150.00   25
  6  \w     39.00  98.00   1.00    1.00    --   43.01-125.00-180.00   59
  7  \w     29.00  64.00   1.00    1.00    --   43.01-125.00 -60.00   35
  8  \w    138.00 177.00   1.00    4.00    --  112.00  15.00  90.00   39
  9  \w     60.00  89.00   1.00    4.00    --  112.00  15.00  90.00   29
 10  \w    100.00 147.00   1.00    4.00    --  112.00 111.00  30.00   47
 11  \w     80.00 178.00   1.00    4.00    --  112.00  77.00-150.00   98
 12  \w     63.00 120.00   1.00    4.00    --  112.00 178.00 120.00   57
 13  \w     83.00 148.00   1.00    4.00    --  112.00  61.00 120.00   65
 14  \w     76.00 104.00   1.00    4.00    --  112.00 -94.00-180.00   28
 15  \w    129.00 178.00   1.00    4.00    --  112.00 111.00 -90.00   49
 16  \w     71.00  99.00   1.00    4.00    --  112.00-111.00 -90.00   28
 17  \w     69.00 112.00   1.00    4.00    --  112.00-111.00 -30.00   43
 18  \w     39.00  65.00   1.00    4.00    --  112.00-111.00 -90.00   26
 19  \w     80.00 113.00   1.00    4.00    --  112.00-111.00  30.00   33
 20  \w     42.00 135.00   1.00    4.00    --  112.00 -45.00-120.00   93
 21  \w     76.00 113.00   1.00    4.00    --  112.00-111.00  90.00   37
 22  \w     37.00 100.00   1.00    4.00    --  112.00-111.00 150.00   63
 23  \w    111.00 137.00   1.00    4.00    --  112.00  61.00 -60.00   26
 24  \w    142.00 168.00   1.00    4.00    --  112.00  61.00 -60.00   26
 25  \w     42.00  83.00   1.00    4.00    --  112.00-111.00-150.00   41
 26  \w    112.00 177.00   1.00    4.00    --  112.00  61.00 -30.00   65
 27  \w     52.00  79.00   1.00    4.00    --  112.00 -77.00-120.00   27
 28  \w    115.00 141.00   1.00    4.00    --  112.00 -77.00-120.00   26
 29  \w     95.00 122.00   1.00    4.00    --  112.00 -77.00   0.00   27
 30  \w    130.00 170.00   1.00    4.00    --  112.00 111.00-180.00   40
 31  \w     63.00  88.00   1.00    4.00    --  112.00 -77.00   0.00   25
;
_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      -0.0161666000
_diffrn_orient_matrix_UB_12      0.1825390000
_diffrn_orient_matrix_UB_13      0.0113888000
_diffrn_orient_matrix_UB_21      -0.0653251000
_diffrn_orient_matrix_UB_22      -0.0144027000
_diffrn_orient_matrix_UB_23      -0.1330485000
_diffrn_orient_matrix_UB_31      -0.1855510000
_diffrn_orient_matrix_UB_32      -0.0216069000
_diffrn_orient_matrix_UB_33      0.0042600000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6988
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.558
_diffrn_reflns_theta_min         3.833
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.588
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.313
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019).
 Numerical absorption correction based on Gaussian integration over
 a multifaceted crystal model.
 Empirical absorption correction using spherical harmonics
 as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            'clear intense orange'
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       prism
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.554
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.077
_refine_diff_density_max         1.208
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         3299
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0492P)^2^+0.7322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.0937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3206
_reflns_number_total             3299
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00049c2.cif
_cod_data_source_block           il-2-250
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7703444--7703450.cif.
;
_cod_database_code               7703445
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C28 H38 Cl2 N6 O4 Pd'
_shelx_estimated_absorpt_t_max   0.631
_shelx_estimated_absorpt_t_min   0.121
_reflns_odcompleteness_completeness 99.79
_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.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C)
;
_shelx_res_checksum              39434
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.946
_oxdiff_exptl_absorpt_empirical_full_min 0.624