Incorporation of coinage metal-NHC complexes into heptaphosphide clusters.
Jo, Minyoung; Li, Jingbai; Dragulescu-Andrasi, Alina; Rogachev, Andrey Yu; Shatruk, Michael; Dalton transactions (Cambridge, England : 2003) 49 (2020) 12955–12959; doi:10.1039/d0dt03119d

data_7705404
_publ_section_title
;
 Incorporation of coinage metal-NHC complexes into heptaphosphide
 clusters.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12955
_journal_page_last               12959
_journal_paper_doi               10.1039/d0dt03119d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C81 H108 Au3 N6 P7, C4 H8 O'
_chemical_formula_sum            'C85 H116 Au3 N6 O P7'
_chemical_formula_weight         2045.52
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-01-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-18 deposited with the CCDC.	2020-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 125.2160(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4686(2)
_cell_length_b                   17.44450(10)
_cell_length_c                   34.2250(3)
_cell_measurement_reflns_used    180436
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      77.6190
_cell_measurement_theta_min      2.7950
_cell_volume                     9008.44(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_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_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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     -7.00  19.00   0.50    1.10    --   47.20 -21.00  14.00   52
  2  \w     64.00  95.00   0.50    4.39    --  107.75 -94.00 -90.00   62
  3  \w     62.00 100.00   0.50    4.39    --  107.75 -94.00 -60.00   76
  4  \w     69.00  99.00   0.50    4.39    --  107.75 -77.00  30.00   60
  5  \w     43.00  70.00   0.50    4.39    --  107.75 -61.00  60.00   54
  6  \w     39.00  71.00   0.50    4.39    --  107.75 -61.00   0.00   64
  7  \w     53.00 105.00   0.50    4.39    --  107.75 -94.00  60.00  104
  8  \w     59.00  98.00   0.50    4.39    --  107.75 -77.00 150.00   78
  9  \w     41.00 104.00   0.50    4.39    --  107.75 -77.00 120.00  126
 10  \w     39.00  70.00   0.50    4.39    --  107.75 -61.00  30.00   62
 11  \w     35.00  60.00   0.50    4.39    --  107.75 -61.00 -30.00   50
 12  \w     35.00  60.00   0.50    4.39    --  107.75 -61.00 -90.00   50
 13  \w     38.00  69.00   0.50    4.39    --  107.75 -77.00-120.00   62
 14  \w     41.00  66.00   0.50    4.39    --  107.75 -94.00-180.00   50
 15  \w     47.00  76.00   0.50    4.39    --  107.75 -77.00-150.00   58
 16  \w     48.00 106.00   0.50    4.39    --  107.75 -94.00-120.00  116
 17  \w     46.00  71.00   0.50    4.39    --  107.75 -61.00-180.00   50
 18  \w     35.00 106.00   0.50    4.39    --  107.75 -94.00-150.00  142
 19  \w     45.00  80.00   0.50    1.10    --   47.20  21.00-178.00   70
 20  \w     98.00 177.00   0.50    4.39    --  107.75  21.00-178.00  158
 21  \w    110.00 136.00   0.50    4.39    --  107.75  45.00 -90.00   52
 22  \w    117.00 175.00   0.50    4.39    --  107.75  15.00-150.00  116
 23  \w     95.00 144.00   0.50    4.39    --  107.75  15.00  90.00   98
 24  \w     98.00 162.00   0.50    4.39    --  107.75  15.00 120.00  128
 25  \w     41.00 101.00   0.50    4.39    --  107.75 -94.00 120.00  120
 26  \w     35.00  70.00   0.50    4.39    --  107.75 -61.00 120.00   70
 27  \w    -28.00  26.00   0.50    1.10    --  -47.20  21.00-178.00  108
 28  \w    -27.00   7.00   0.50    1.10    --  -47.20  19.00 -30.00   68
 29  \w    -44.00 -17.00   0.50    4.39    --  -86.25  45.00 -30.00   54
 30  \w    -48.00 -15.00   0.50    4.39    --  -86.25  45.00  30.00   66
 31  \w   -123.00 -38.00   0.50    1.10    --  -47.20 -21.00  14.00  170
 32  \w   -138.00-113.00   0.50    4.39    --  -86.25 -21.00  14.00   50
 33  \w    -84.00 -18.00   0.50    1.10    --  -47.20 125.00-180.00  132
 34  \w   -110.00 -35.00   0.50    1.10    --  -47.20 -19.00 120.00  150
 35  \w   -119.00 -35.00   0.50    1.10    --  -47.20 -43.00-110.15  168
 36  \w    -70.00 -34.00   0.50    1.10    --  -47.20 -43.00 149.38   72
 37  \w    -63.00 -34.00   0.50    1.10    --  -47.20 -44.00 100.42   58
 38  \w    -82.00 -34.00   0.50    1.10    --  -47.20 -45.00 -15.55   96
 39  \w    -68.00 -32.00   0.50    1.10    --  -47.20 -57.00  90.00   72
 40  \w    -50.00 -24.00   0.50    1.10    --  -47.20 -77.00 -90.00   52
 41  \w    -55.00 -28.00   0.50    1.10    --  -47.20 -67.00  30.07   54
 42  \w     78.00 109.00   0.50    1.10    --   47.20  77.00 120.00   62
 43  \w     25.00  55.00   0.50    1.10    --   47.20  77.00  30.00   60
 44  \w     32.00  59.00   0.50    1.10    --   47.20  57.00-120.00   54
 45  \w     25.00  58.00   0.50    1.10    --   47.20  77.00  90.00   66
 46  \w     37.00 106.00   0.50    1.10    --   47.20  37.00-120.00  138
 47  \w     25.00  55.00   0.50    1.10    --   47.20  77.00-120.00   60
 48  \w     34.00  93.00   0.50    1.10    --   47.20-125.00  30.00  118
 49  \w     25.00  64.00   0.50    1.10    --   47.20  77.00 -60.00   78
 50  \w     25.00  56.00   0.50    1.10    --   47.20  77.00 150.00   62
 51  \w     25.00  50.00   0.50    1.10    --   47.20  77.00   0.00   50
 52  \w     49.00  94.00   0.50    1.10    --   47.20-125.00-120.00   90
 53  \w     26.00  51.00   0.50    1.10    --   47.20  77.00 120.00   50
 54  \w     25.00  71.00   0.50    1.10    --   47.20  77.00-180.00   92
 55  \w    -92.00 -64.00   0.50    4.39    --  -86.25 -76.00 106.11   56
 56  \w    -87.00 -62.00   0.50    4.39    --  -86.25 -79.00  45.04   50
 57  \w    -88.00 -63.00   0.50    4.39    --  -86.25 -77.00-120.00   50
 58  \w    -88.00 -62.00   0.50    4.39    --  -86.25 -79.00 137.74   52
 59  \w    -89.00 -63.00   0.50    4.39    --  -86.25 -77.00-102.10   52
 60  \w    -87.00 -62.00   0.50    4.39    --  -86.25 -79.00 -90.39   50
 61  \w    -91.00 -64.00   0.50    4.39    --  -86.25 -75.00  95.82   54
 62  \w    -88.00 -63.00   0.50    4.39    --  -86.25 -78.00 -48.39   50
 63  \w    -88.00 -62.00   0.50    4.39    --  -86.25 -80.00 130.20   52
 64  \w   -155.00-122.00   0.50    4.39    --  -86.25 -79.00 137.74   66
 65  \w    -88.00 -62.00   0.50    4.39    --  -86.25 -79.00 -76.87   52
 66  \w    -88.00 -63.00   0.50    4.39    --  -86.25 -77.00 -44.00   50
 67  \w    -91.00 -65.00   0.50    4.39    --  -86.25 -72.00  72.95   52
 68  \w   -148.00-122.00   0.50    4.39    --  -86.25 -79.00 -76.87   52
 69  \w    -87.00 -62.00   0.50    4.39    --  -86.25 -80.00 169.50   50
 70  \w    -98.00 -64.00   0.50    4.39    --  -86.25 -75.00-140.69   68
 71  \w   -102.00 -63.00   0.50    4.39    --  -86.25 -77.00 -30.00   78
 72  \w    -89.00 -64.00   0.50    4.39    --  -86.25 -75.00-160.73   50
 73  \w    -89.00 -63.00   0.50    4.39    --  -86.25 -77.00   0.00   52
 74  \w    -90.00 -64.00   0.50    4.39    --  -86.25 -76.00-172.04   52
 75  \w    -88.00 -62.00   0.50    4.39    --  -86.25 -80.00 -58.38   52
 76  \w    -89.00 -63.00   0.50    4.39    --  -86.25 -77.00  17.91   52
 77  \w    -89.00 -63.00   0.50    4.39    --  -86.25 -77.00  30.00   52
 78  \w    -88.00 -63.00   0.50    4.39    --  -86.25 -77.00-180.00   50
 79  \w   -104.00 -62.00   0.50    4.39    --  -86.25 -80.00  -4.76   84
 80  \w    -88.00 -62.00   0.50    4.39    --  -86.25 -80.00 156.76   52
 81  \w    -90.00 -64.00   0.50    4.39    --  -86.25 -76.00  51.59   52
 82  \w    -89.00 -64.00   0.50    4.39    --  -86.25 -76.00  62.32   50
 83  \w    -89.00 -63.00   0.50    4.39    --  -86.25 -77.00  90.00   52
 84  \w     73.00 107.00   0.50    4.39    --  107.75-105.00  21.17   68
 85  \w     93.00 120.00   0.50    4.39    --  107.75  61.00  30.00   54
 86  \w     37.00  66.00   0.50    4.39    --  107.75-105.00  21.17   58
 87  \w     85.00 114.00   0.50    4.39    --  107.75  77.00-120.00   58
 88  \w    130.00 170.00   0.50    4.39    --  107.75  75.00  -8.46   80
 89  \w     86.00 125.00   0.50    4.39    --  107.75  77.00 120.00   78
 90  \w     86.00 111.00   0.50    4.39    --  107.75  75.00  -8.46   50
 91  \w    129.00 174.00   0.50    4.39    --  107.75  77.00-120.00   90
 92  \w    143.00 172.00   0.50    4.39    --  107.75  77.00   0.00   58
 93  \w    139.00 175.00   0.50    4.39    --  107.75  61.00  30.00   72
 94  \w     85.00 121.00   0.50    4.39    --  107.75  77.00  90.00   72
 95  \w    135.00 161.00   0.50    4.39    --  107.75  77.00  90.00   52
 96  \w     85.00 125.00   0.50    4.39    --  107.75  77.00   0.00   80
 97  \w     84.00 159.00   0.50    4.39    --  107.75  79.00 -49.87  150
 98  \w     85.00 143.00   0.50    4.39    --  107.75  77.00 -90.00  116
 99  \w     81.00 107.00   0.50    4.39    --  107.75-109.00-107.35   52
100  \w    124.00 164.00   0.50    4.39    --  107.75  80.00 -69.68   80
101  \w     85.00 116.00   0.50    4.39    --  107.75-131.00 134.57   62
102  \w     38.00  81.00   0.50    4.39    --  107.75-131.00 134.57   86
103  \w     86.00 120.00   0.50    4.39    --  107.75  80.00 -69.68   68
104  \w     36.00 106.00   0.50    4.39    --  107.75 -94.00  30.00  140
105  \w    136.00 168.00   0.50    4.39    --  107.75  77.00 150.00   64
106  \w     85.00 171.00   0.50    4.39    --  107.75  77.00 -30.00  172
107  \w     97.00 124.00   0.50    4.39    --  107.75-141.00-120.95   54
108  \w     48.00  75.00   0.50    4.39    --  107.75-141.00-120.95   54
109  \w     83.00 108.00   0.50    4.39    --  107.75-113.00 -34.30   50
110  \w     94.00 144.00   0.50    4.39    --  107.75  61.00-120.00  100
111  \w     72.00 102.00   0.50    4.39    --  107.75 -94.00 -30.00   60
112  \w     35.00  77.00   0.50    4.39    --  107.75-113.00 -34.30   84
113  \w    136.00 178.00   0.50    4.39    --  107.75  77.00  30.00   84
114  \w    128.00 162.00   0.50    4.39    --  107.75  61.00 150.00   68
115  \w     87.00 120.00   0.50    4.39    --  107.75  77.00  30.00   66
116  \w     92.00 118.00   0.50    4.39    --  107.75  61.00 150.00   52
117  \w     92.00 175.00   0.50    4.39    --  107.75  61.00 120.00  166
118  \w     91.00 168.00   0.50    4.39    --  107.75  61.00 -90.00  154
119  \w    101.00 176.00   0.50    4.39    --  107.75  15.00  30.00  150
120  \w     85.00 111.00   0.50    4.39    --  107.75-125.00 -60.00   52
121  \w    142.00 168.00   0.50    4.39    --  107.75  66.00-144.63   52
122  \w     87.00 128.00   0.50    4.39    --  107.75  77.00 -60.00   82
123  \w    138.00 178.00   0.50    4.39    --  107.75  77.00 -60.00   80
124  \w     37.00  76.00   0.50    4.39    --  107.75-125.00 -60.00   78
125  \w     90.00 116.00   0.50    4.39    --  107.75  66.00-144.63   52
126  \w     85.00 111.00   0.50    4.39    --  107.75-125.00 150.00   52
127  \w     85.00 111.00   0.50    4.39    --  107.75  77.00 150.00   52
128  \w     39.00  64.00   0.50    4.39    --  107.75-125.00 150.00   50
129  \w    151.00 177.00   0.50    4.39    --  107.75  80.00 161.84   52
130  \w     35.00  95.00   0.50    4.39    --  107.75 -77.00 -30.00  120
131  \w     36.00 108.00   0.50    4.39    --  107.75-116.00  -6.68  144
132  \w     84.00 115.00   0.50    4.39    --  107.75  80.00 161.84   62
133  \w    140.00 166.00   0.50    4.39    --  107.75  77.00  60.00   52
134  \w     85.00 125.00   0.50    4.39    --  107.75  77.00  60.00   80
135  \w     85.00 159.00   0.50    4.39    --  107.75  77.00-150.00  148
136  \w    134.00 177.00   0.50    4.39    --  107.75  64.00  61.54   86
137  \w    125.00 151.00   0.50    4.39    --  107.75  77.00-180.00   52
138  \w     91.00 142.00   0.50    4.39    --  107.75  61.00  90.00  102
139  \w    149.00 176.00   0.50    4.39    --  107.75  61.00  90.00   54
140  \w     90.00 117.00   0.50    4.39    --  107.75  64.00  61.54   54
141  \w     85.00 120.00   0.50    4.39    --  107.75  77.00-180.00   70
142  \w    135.00 161.00   0.50    4.39    --  107.75  61.00 -60.00   52
143  \w    140.00 170.00   0.50    4.39    --  107.75  78.00-169.66   60
144  \w     92.00 123.00   0.50    4.39    --  107.75  61.00 -60.00   62
145  \w     86.00 118.00   0.50    4.39    --  107.75  78.00-169.66   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1017218000
_diffrn_orient_matrix_UB_12      -0.0033138000
_diffrn_orient_matrix_UB_13      0.0282853000
_diffrn_orient_matrix_UB_21      0.0084013000
_diffrn_orient_matrix_UB_22      0.0236502000
_diffrn_orient_matrix_UB_23      0.0458328000
_diffrn_orient_matrix_UB_31      -0.0016318000
_diffrn_orient_matrix_UB_32      -0.0850129000
_diffrn_orient_matrix_UB_33      0.0116666000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1845
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            331734
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.251
_diffrn_reflns_theta_min         2.809
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.520
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23014
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       block
_exptl_crystal_F_000             4072
_exptl_crystal_recrystallization_method 'Slow evaporation of THF solution'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.587
_refine_diff_density_min         -1.808
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     943
_refine_ls_number_reflns         19133
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+15.6964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18139
_reflns_number_total             19133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03119d2.cif
_cod_data_source_block           Au-NHC-P7
_cod_depositor_comments
'Adding full bibliography for 7705403--7705404.cif.'
_cod_original_cell_volume        9008.43(16)
_cod_database_code               7705404
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C85 H116 Au3 N7 P7'
_chemical_oxdiff_usercomment     '150 K'
_diffrn_oxdiff_digest_frames
;
019462e76349aa950f8a7cbeac0e61e7f310928c5a3
;
_diffrn_oxdiff_digest_hkl
;
01eb776b62c64fe8eb5688e73840b24b0836f9
;
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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 Ternary CH refined with riding coordinates:
 C37(H37), C49(H49), C40(H40), C22(H22), C67(H67), C52(H52), C10(H10),
 C79(H79), C76(H76), C64(H64), C13(H13), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C82(H82A,H82B), C85(H85A,H85B), C83(H83A,H83B), C84(H84A,H84B)
2.c Aromatic/amide H refined with riding coordinates:
 C56(H56), C3(H3), C57(H57), C30(H30), C2(H2), C34(H34), C29(H29), C35(H35),
 C60(H60), C8(H8), C47(H47), C61(H61), C45(H45), C46(H46), C72(H72), C20(H20),
 C19(H19), C33(H33), C62(H62), C74(H74), C73(H73), C18(H18), C6(H6), C7(H7)
2.d Idealised Me refined as rotating group:
 C65(H65A,H65B,H65C), C53(H53A,H53B,H53C), C38(H38A,H38B,H38C), C77(H77A,H77B,
 H77C), C78(H78A,H78B,H78C), C66(H66A,H66B,H66C), C51(H51A,H51B,H51C), C54(H54A,
 H54B,H54C), C24(H24A,H24B,H24C), C42(H42A,H42B,H42C), C23(H23A,H23B,H23C),
 C41(H41A,H41B,H41C), C80(H80A,H80B,H80C), C50(H50A,H50B,H50C), C12(H12A,H12B,
 H12C), C27(H27A,H27B,H27C), C68(H68A,H68B,H68C), C81(H81A,H81B,H81C), C11(H11A,
 H11B,H11C), C14(H14A,H14B,H14C), C26(H26A,H26B,H26C), C15(H15A,H15B,H15C),
 C39(H39A,H39B,H39C), C69(H69A,H69B,H69C)
;
_shelx_res_checksum              59633
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 4.471
_oxdiff_exptl_absorpt_empirical_full_min 0.203