Phosphine-substituted 1,2,3-triazoles as P,C- and P,N-ligands for photoluminescent coinage metal complexes.
Seifert, Tim P.; Bestgen, Sebastian; Feuerstein, Thomas J.; Lebedkin, Sergei; Krämer, Felix; Fengler, Christian; Gamer, Michael T.; Kappes, Manfred M.; Roesky, Peter W.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15427–15434; doi:10.1039/c9dt01239g

data_7701633
_publ_section_title
;
 Phosphine-substituted 1,2,3-triazoles as P,C- and P,N-ligands for
 photoluminescent coinage metal complexes.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15427
_journal_page_last               15434
_journal_paper_doi               10.1039/c9dt01239g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'C21 H18 Au Cl N3 P, 0.65(C1 H2 Cl2), 0.35(C4 H8 S)'
_chemical_formula_sum            'C23.05 H22.1 Au Cl2.3 N3 P S0.35'
_chemical_formula_weight         661.83
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-04-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-18 deposited with the CCDC.	2019-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   10.9905(2)
_cell_length_b                   10.9905(2)
_cell_length_c                   34.6093(8)
_cell_measurement_reflns_used    23581
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.85
_cell_measurement_theta_min      1.77
_cell_volume                     3620.41(13)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
PLATON (A.L.Spek, 2009)
;
_computing_data_collection       'X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)'
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
PLATON (A.L.Spek, 2009)
;
_computing_molecular_graphics    'Diamond 4, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
MS Word (Microsoft)
Olex2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus100K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 100K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_details
;
 883 frames, detector distance = 80 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            22207
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.970
_diffrn_reflns_theta_min         1.765
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    6.462
_exptl_absorpt_correction_T_max  0.4509
_exptl_absorpt_correction_T_min  0.0019
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "Crystallographic Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_description       block
_exptl_crystal_F_000             1921
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.154
_refine_diff_density_max         1.822
_refine_diff_density_min         -0.948
_refine_diff_density_rms         0.178
_refine_ls_abs_structure_details
;
 Flack x determined using 2003 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5723
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0574P)^2^+6.1249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1056
_reflns_Friedel_coverage         0.714
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.873
_reflns_number_gt                5205
_reflns_number_total             5723
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01239g2.cif
_cod_data_source_block           tps241
_cod_original_cell_volume        3620.41(16)
_cod_original_formula_sum        'C23.05 H22.10 Au Cl2.30 N3 P S0.35'
_cod_database_code               7701633
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.436
_shelx_estimated_absorpt_t_min   0.208
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl2-C24
 1.79 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl3B \\sim C25B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
S \\sim C22 \\sim C23: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Cl2 \\sim C24: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Others
 Fixed Sof: Cl3A(0.7) C25A(0.35) H25A(0.35) H25B(0.35) Cl2(0.3) C24(0.15)
 H24A(0.15) H24B(0.15) Cl3B(0.3) C25B(0.15) H25C(0.15) H25D(0.15) S(0.35)
 C22(0.7) H22A(0.7) H22B(0.7) C23(0.7) H23A(0.7) H23B(0.7)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C25A(H25A,H25B), C24(H24A,H24B), C25B(H25C,H25D), C22(H22A,H22B),
  C23(H23A,H23B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21)
;
_shelx_res_checksum              41852
_olex2_submission_special_instructions 'No special instructions were received'