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_7703444
_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         'C22 H30 Cl2 N6 Pd'
_chemical_formula_sum            'C22 H30 Cl2 N6 Pd'
_chemical_formula_weight         555.82
_chemical_name_common            (TolTr)2PdCl2
_chemical_name_systematic        AS868
_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             2019-04-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-04 deposited with the CCDC.	2020-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                82.298(9)
_cell_angle_beta                 68.456(10)
_cell_angle_gamma                70.100(10)
_cell_formula_units_Z            2
_cell_length_a                   9.2984(10)
_cell_length_b                   12.1013(13)
_cell_length_c                   12.2378(13)
_cell_measurement_reflns_used    3328
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.6280
_cell_measurement_theta_min      3.8500
_cell_volume                     1204.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.20a (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      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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    -55.00  35.00   1.00    4.00    --  -40.66  77.00 120.00   90
  2  \w   -113.00 -14.00   1.00    4.00    --  -40.66 -57.00   0.00   99
  3  \w    -41.00 -15.00   1.00    4.00    --  -40.66  57.00   0.00   26
  4  \w     46.00  95.00   1.00    4.00    --   40.66-125.00 -60.00   49
  5  \w     14.00  63.00   1.00    4.00    --   40.66  57.00-120.00   49
  6  \w     44.00 115.00   1.00    4.00    --   40.66  38.00 -90.00   71
  7  \w     44.00 134.00   1.00   16.00    --  107.03 -61.00 -30.00   90
  8  \w     82.00 178.00   1.00   16.00    --  107.03  61.00 -60.00   96
  9  \w     86.00 117.00   1.00   16.00    --  107.03-125.00-180.00   31
 10  \w    105.00 169.00   1.00   16.00    --  107.03 125.00-120.00   64
 11  \w     77.00 104.00   1.00   16.00    --  107.03-125.00  30.00   27
 12  \w     83.00 156.00   1.00   16.00    --  107.03  45.00   0.00   73
 13  \w     43.00  78.00   1.00   16.00    --  107.03 -94.00-180.00   35
 14  \w    101.00 157.00   1.00   16.00    --  107.03  30.00  90.00   56
 15  \w     34.00 130.00   1.00   16.00    --  107.03 -45.00 150.00   96
 16  \w     90.00 117.00   1.00   16.00    --  107.03-125.00  90.00   27
 17  \w     36.00  61.00   1.00   16.00    --  107.03-125.00  90.00   25
 18  \w     55.00 140.00   1.00   16.00    --  107.03 -77.00-150.00   85
 19  \w     44.00  71.00   1.00   16.00    --  107.03-125.00-180.00   27
 20  \w     93.00 118.00   1.00   16.00    --  107.03-125.00 -60.00   25
 21  \w    102.00 167.00   1.00   16.00    --  107.03  15.00  60.00   65
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1390341000
_diffrn_orient_matrix_UB_12      0.1168539000
_diffrn_orient_matrix_UB_13      0.0095779000
_diffrn_orient_matrix_UB_21      -0.0974579000
_diffrn_orient_matrix_UB_22      -0.0370814000
_diffrn_orient_matrix_UB_23      0.1226703000
_diffrn_orient_matrix_UB_31      0.0801049000
_diffrn_orient_matrix_UB_32      0.0574672000
_diffrn_orient_matrix_UB_33      0.0563873000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_unetI/netI     0.0856
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7530
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        66.580
_diffrn_reflns_theta_max         66.580
_diffrn_reflns_theta_min         3.884
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.423
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.214
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.20a (Rigaku Oxford Diffraction, 2018).
 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    1.533
_exptl_crystal_description       prism
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.101
_refine_diff_density_max         2.430
_refine_diff_density_min         -1.475
_refine_diff_density_rms         0.276
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         4181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_gt           0.0935
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1631P)^2^+2.7798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2469
_refine_ls_wR_factor_ref         0.2614
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3447
_reflns_number_total             4181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00049c2.cif
_cod_data_source_block           as868
_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               7703444
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C22 H30 N6 Cl2 Pd1'
_reflns_odcompleteness_completeness 98.44
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C12(H12A,H12B), C13(H13A,
 H13B), C14(H14A,H14B), C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C9(H9), C10(H10), C17(H17), C18(H18), C20(H20), C21(H21)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C22(H22A,H22B,H22C)
;
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 12.428
_oxdiff_exptl_absorpt_empirical_full_min 0.187