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_7701636
_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
'0.5(C44 H42 Au2 Cl2 N6 P2), C F3 O3 S, 0.75(C H2 Cl2)'
_chemical_formula_sum            'C23.75 H22.5 Au Cl2.5 F3 N3 O3 P S'
_chemical_formula_weight         803.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 104.362(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.5105(5)
_cell_length_b                   11.1318(2)
_cell_length_c                   23.4398(6)
_cell_measurement_reflns_used    46735
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.71
_cell_measurement_theta_min      1.80
_cell_volume                     5690.0(2)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_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      150
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
 134 frames, detector distance = 100 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_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  0.0265
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            33022
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.527
_diffrn_reflns_theta_min         1.794
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    5.587
_exptl_absorpt_correction_T_max  0.4786
_exptl_absorpt_correction_T_min  0.1337
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_description       needle
_exptl_crystal_F_000             3116
_exptl_crystal_size_max          0.483
_exptl_crystal_size_mid          0.353
_exptl_crystal_size_min          0.192
_refine_diff_density_max         1.634
_refine_diff_density_min         -1.194
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         15774
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0316P)^2^+21.5241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13642
_reflns_number_total             15774
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01239g2.cif
_cod_data_source_block           tps_pmetriazaucl
_cod_original_formula_sum        'C23.75 H22.50 Au Cl2.50 F3 N3 O3 P S'
_cod_database_code               7701636
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.413
_shelx_estimated_absorpt_t_min   0.173
_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. Restrained distances
 Cl5-C48 = Cl6-C48
 1.771 with sigma of 0.01
 Cl5-Cl6
 2.916 with sigma of 0.03
3. Uiso/Uaniso restraints and constraints
C28 \\sim C27 \\sim C32 \\sim C31 \\sim C30 \\sim C29 \\sim C26: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04
Cl5 \\sim Cl6 \\sim C48: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Cl5, Cl6, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Cl5(0.5) Cl6(0.5) C48(0.5) H48A(0.5) H48B(0.5)
6.a Free rotating group:
 Cl5(Cl6,C48)
6.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C26(H26A,H26B), C47(H47A,H47B), C48(H48A,H48B)
6.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C2(H2), C20(H20), C44(H44), C35(H35), C13(H13), C21(H21), C37(H37),
 C14(H14), C16(H16), C24(H24), C38(H38), C7(H7), C19(H19), C34(H34), C22(H22),
 C36(H36), C12(H12), C10(H10), C6(H6), C8(H8), C40(H40), C9(H9), C15(H15),
 C32(H32), C31(H31), C30(H30), C29(H29), C28(H28), C42(H42), C41(H41), C43(H43)
6.d Fitted hexagon refined as free rotating group:
 C27(C32,C31,C30,C29,C28)
6.e Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              85373
_olex2_submission_special_instructions 'No special instructions were received'