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_7701632
_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
'C50 H52 Au2 Cl2 Cu N6 O2 P2, F6 P, 2(C4 H8 O)'
_chemical_formula_sum            'C58 H68 Au2 Cl2 Cu F6 N6 O4 P3'
_chemical_formula_weight         1648.46
_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
_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                 92.509(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3665(4)
_cell_length_b                   27.9101(11)
_cell_length_c                   21.4135(7)
_cell_measurement_reflns_used    28404
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      1.46
_cell_volume                     6189.6(4)
_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                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.809
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0839
_diffrn_reflns_av_unetI/netI     0.0812
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.809
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            34254
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.809
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.066
_diffrn_reflns_theta_min         1.459
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    5.33
_exptl_absorpt_correction_T_max  0.4780
_exptl_absorpt_correction_T_min  0.1678
_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    1.769
_exptl_crystal_description       block
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.413
_exptl_crystal_size_mid          0.329
_exptl_crystal_size_min          0.251
_refine_diff_density_max         2.906
_refine_diff_density_min         -1.569
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         14732
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.1263
_refine_ls_R_factor_gt           0.0831
_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^)+(0.0505P)^2^+288.1349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2095
_refine_ls_wR_factor_ref         0.2401
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9808
_reflns_number_total             14732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01239g2.cif
_cod_data_source_block           tps263
_cod_database_code               7701632
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.350
_shelx_estimated_absorpt_t_min   0.218
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9307(10)
 0.0693(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
3. Restrained distances
 O4B-C55B \\sim O4B-C58
 with sigma of 0.02
 O4A-C55A \\sim O4A-C58
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O3A \\sim C51A \\sim C52A \\sim C53A \\sim C54A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
O3B \\sim C51B \\sim C52B \\sim C53B \\sim C54B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
P3 \\sim F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6: within 2A with sigma
of 0.008 and sigma for terminal atoms of 0.016
O4A \\sim O4B: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
C57 \\sim O4B \\sim C55B \\sim C56B: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
5. Others
 Fixed Sof: H57A(0.75) H57B(0.75) H57C(0.25) H57D(0.25) H58C(0.25) H58D(0.25)
 H58A(0.75) H58B(0.75) O4A(0.75) C55A(0.75) H55A(0.75) H55B(0.75) C56A(0.75)
 H56A(0.75) H56B(0.75) O4B(0.25) C55B(0.25) H55C(0.25) H55D(0.25) C56B(0.25)
 H56C(0.25) H56D(0.25) O3A(0.66667) C51A(0.66667) H51A(0.66667) H51B(0.66667)
 C52A(0.66667) H52A(0.66667) H52B(0.66667) C53A(0.66667) H53A(0.66667)
 H53B(0.66667) C54A(0.66667) H54A(0.66667) H54B(0.66667) O3B(0.33333)
 C51B(0.33333) H51C(0.33333) H51D(0.33333) C52B(0.33333) H52C(0.33333)
 H52D(0.33333) C53B(0.33333) H53C(0.33333) H53D(0.33333) C54B(0.33333)
 H54C(0.33333) H54D(0.33333)
6.a Free rotating group:
 O3A(C51A,C52A,C53A), O3B(C51B,C52B,C53B,C54B)
6.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C24(H24A,H24B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B),
 C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B),
  C57(H57A,H57B), C57(H57C,H57D), C58(H58C,H58D), C58(H58A,H58B), C55A(H55A,
 H55B), C56A(H56A,H56B), C55B(H55C,H55D), C56B(H56C,H56D), C51A(H51A,H51B),
 C52A(H52A,H52B), C53A(H53A,H53B), C54A(H54A,H54B), C51B(H51C,H51D), C52B(H52C,
 H52D), C53B(H53C,H53D), C54B(H54C,H54D)
6.c 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), C23(H23),
  C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42)
;
_shelx_res_checksum              57231
_olex2_submission_special_instructions 'No special instructions were received'