Synthesis of hydroxyl-functionalized N-heterocyclic carbene gold(i) complexes and peptide conjugates.
Diehl, Tobias; Krause, Melanie T. S.; Ueberlein, Sven; Becker, Stefanie; Trommer, Aline; Schnakenburg, Gregor; Engeser, Marianne; Dalton transactions (Cambridge, England : 2003) 46 (2017) 2988–2997; doi:10.1039/c6dt04834j

data_7042008
_publ_section_title
;
 Synthesis of hydroxyl-functionalized N-heterocyclic carbene gold(i)
 complexes and peptide conjugates.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2988
_journal_page_last               2997
_journal_paper_doi               10.1039/c6dt04834j
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C16 H28 Au N4 O2, F6 P'
_chemical_formula_sum            'C16 H28 Au F6 N4 O2 P'
_chemical_formula_weight         650.36
_chemical_name_systematic        TD43
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d'
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-01-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_audit_update_record
;
2017-01-18 deposited with the CCDC.
2017-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   13.6194(6)
_cell_length_b                   17.9428(9)
_cell_length_c                   36.8915(17)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.610
_cell_measurement_theta_min      2.503
_cell_volume                     9015.2(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'ApexII detector'
_diffrn_detector_area_resol_mean 8
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            31712
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         3.339
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.667
_exptl_absorpt_correction_T_max  0.7990
_exptl_absorpt_correction_T_min  0.3554
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 
0.0830 before and 0.0509 after correction. The Ratio of minimum to maximum 
transmission is 0.4448. The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.917
_exptl_crystal_description       plate
_exptl_crystal_F_000             5056
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.337
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2468
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0238
_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^)+(0.0244P)^2^+72.1746P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0590
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2068
_reflns_number_total             2468
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04834j2.cif
_cod_data_source_block           4859f
_cod_depositor_comments
'Adding full bibliography for 7042003--7042010.cif.'
_cod_database_code               7042008
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.776
_shelx_estimated_absorpt_t_min   0.284
_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, All O(H) groups
2. Rigid body (RIGU) restrains
 F2, F3, F2A, P1, F3A, F1, F4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(F2A)=Sof(F3A)=1-FVAR(1)
 Sof(F2)=Sof(F3)=FVAR(1)
 Fixed Sof: H1A(0.5) H1B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3)
4.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
4.d Idealised tetrahedral OH refined as rotating group:
 O1(H1A), O1(H1B)
;
_shelx_res_checksum              10336
_olex2_submission_special_instructions 'No special instructions were received'