Synthesis of an expanded pincer ligand and its bimetallic coinage metal complexes.
Delaney, Andie R.; Yu, Li-Juan; Coote, Michelle L.; Colebatch, Annie L.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 11909–11917; doi:10.1039/d1dt01741a

data_7707973
_publ_section_title
;
 Synthesis of an expanded pincer ligand and its bimetallic coinage metal
 complexes.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11909
_journal_page_last               11917
_journal_paper_doi               10.1039/d1dt01741a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C24 H40 Ag2 Cl2 N2 O2 P2, 2(C2 H3 N)'
_chemical_formula_sum            'C28 H46 Ag2 Cl2 N4 O2 P2'
_chemical_formula_weight         819.27
_chemical_name_systematic        tBuPONNOPAg2Cl2
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-05-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-27 deposited with the CCDC.	2021-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.463(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.2144(4)
_cell_length_b                   9.5605(3)
_cell_length_c                   15.3894(3)
_cell_measurement_reflns_used    7926
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      70.6680
_cell_measurement_theta_min      7.2640
_cell_volume                     1795.45(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_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    -54.00  29.00   1.00    1.00    --  -36.03  38.00 -30.00   83
  2  \w    -81.00 -40.00   1.00    1.00    --  -36.03 125.00 -60.00   41
  3  \w    -49.00  28.00   1.00    1.00    --  -36.03  57.00-150.00   77
  4  \w    -53.00  30.00   1.00    1.00    --  -36.03  57.00 120.00   83
  5  \w    -65.00 -19.00   1.00    1.00    --  -36.03 -57.00 -30.00   46
  6  \w   -102.00 -22.00   1.00    1.00    --  -36.03 -57.00-120.00   80
  7  \w      4.00  29.00   1.00    1.00    --   36.03  86.00 177.06   25
  8  \w     43.00  89.00   1.00    1.00    --   36.03  57.00-120.00   46
  9  \w     46.00  95.00   1.00    1.00    --   36.03  71.00  74.66   49
 10  \w      2.00  28.00   1.00    1.00    --   36.03  90.00 124.76   26
 11  \w     10.00  41.00   1.00    1.00    --   36.03  77.00  -9.47   31
 12  \w     13.00  44.00   1.00    1.00    --   36.03  71.00  74.66   31
 13  \w     54.00  89.00   1.00    1.00    --   36.03-125.00-120.00   35
 14  \w     69.00  96.00   1.00    1.00    --   36.03  38.00-150.00   27
 15  \w     22.00  77.00   1.00    1.00    --   36.03  57.00-150.00   55
 16  \w     11.00  39.00   1.00    1.00    --   36.03  76.00 -98.82   28
 17  \w     17.00 102.00   1.00    1.00    --   36.03  38.00   0.00   85
 18  \w    -32.00  52.00   1.00    1.00    --   36.03 -38.00 -30.00   84
 19  \w     14.00  80.00   1.00    1.00    --   36.03  19.00 120.00   66
 20  \w     23.00  81.00   1.00    1.00    --   36.03  57.00 150.00   58
 21  \w      4.00  31.00   1.00    1.00    --   36.03  86.00 -33.15   27
 22  \w     18.00  51.00   1.00    1.00    --   36.03  38.00-150.00   33
 23  \w    131.00 172.00   1.00    1.27    --  105.15  61.00 150.00   41
 24  \w    131.00 171.00   1.00    1.27    --  105.15  61.00  30.00   40
 25  \w     87.00 118.00   1.00    1.27    --  105.15  61.00 150.00   31
 26  \w     87.00 114.00   1.00    1.27    --  105.15  61.00  30.00   27
 27  \w     36.00 106.00   1.00    1.27    --  105.15 -95.00   0.00   70
 28  \w     88.00 121.00   1.00    1.27    --  105.15  45.00-120.00   33
 29  \w     84.00 111.00   1.00    1.27    --  105.15  30.00 120.00   27
 30  \w     88.00 113.00   1.00    1.27    --  105.15  61.00  90.00   25
 31  \w     87.00 170.00   1.00    1.27    --  105.15  61.00 -90.00   83
 32  \w    137.00 164.00   1.00    1.27    --  105.15  61.00  60.00   27
 33  \w    132.00 167.00   1.00    1.27    --  105.15  61.00 120.00   35
 34  \w     88.00 114.00   1.00    1.27    --  105.15  45.00 -60.00   26
 35  \w     87.00 113.00   1.00    1.27    --  105.15  61.00 120.00   26
 36  \w     87.00 114.00   1.00    1.27    --  105.15  61.00  60.00   27
 37  \w    132.00 170.00   1.00    1.27    --  105.15  61.00-180.00   38
 38  \w     87.00 113.00   1.00    1.27    --  105.15  61.00-180.00   26
 39  \w     89.00 123.00   1.00    1.27    --  105.15  45.00-150.00   34
 40  \w     87.00 121.00   1.00    1.27    --  105.15  61.00-150.00   34
 41  \w     88.00 114.00   1.00    1.27    --  105.15  45.00 120.00   26
 42  \w     67.00 106.00   1.00    1.27    --  105.15 -95.00 150.00   39
 43  \w    130.00 171.00   1.00    1.27    --  105.15  61.00-150.00   41
 44  \w     89.00 114.00   1.00    1.27    --  105.15  45.00  90.00   25
 45  \w    118.00 145.00   1.00    1.27    --  105.15  45.00  90.00   27
 46  \w     88.00 125.00   1.00    1.27    --  105.15  45.00 -90.00   37
 47  \w     36.00  64.00   1.00    1.27    --  105.15 -95.00 150.00   28
 48  \w     56.00 108.00   1.00    1.27    --  105.15-111.00 -30.00   52
 49  \w     88.00 113.00   1.00    1.27    --  105.15  61.00 -60.00   25
 50  \w    133.00 171.00   1.00    1.27    --  105.15  61.00 -60.00   38
 51  \w     36.00  65.00   1.00    1.27    --  105.15 -95.00-150.00   29
 52  \w     77.00 104.00   1.00    1.27    --  105.15 -95.00-150.00   27
 53  \w     56.00 122.00   1.00    1.27    --  105.15 -61.00-180.00   66
 54  \w     41.00  68.00   1.00    1.27    --  105.15 -95.00-180.00   27
 55  \w     88.00 122.00   1.00    1.27    --  105.15  45.00 -30.00   34
 56  \w     85.00 110.00   1.00    1.27    --  105.15  30.00-150.00   25
 57  \w     85.00 112.00   1.00    1.27    --  105.15  30.00  90.00   27
 58  \w     89.00 121.00   1.00    1.27    --  105.15  45.00-180.00   32
 59  \w     88.00 147.00   1.00    1.27    --  105.15  45.00   0.00   59
 60  \w     88.00 171.00   1.00    1.27    --  105.15  61.00   0.00   83
 61  \w     88.00 121.00   1.00    1.27    --  105.15  45.00 150.00   33
 62  \w    137.00 164.00   1.00    1.27    --  105.15  61.00 -30.00   27
 63  \w     88.00 114.00   1.00    1.27    --  105.15  45.00  60.00   26
 64  \w     39.00 117.00   1.00    1.27    --  105.15 -61.00   0.00   78
 65  \w    141.00 172.00   1.00    1.27    --  105.15  61.00-120.00   31
 66  \w     87.00 114.00   1.00    1.27    --  105.15  61.00-120.00   27
 67  \w    119.00 172.00   1.00    1.27    --  105.15  61.00  90.00   53
 68  \w     70.00 105.00   1.00    1.27    --  105.15 -95.00  90.00   35
 69  \w     87.00 124.00   1.00    1.27    --  105.15  61.00 -30.00   37
 70  \w     88.00 114.00   1.00    1.27    --  105.15  45.00  30.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0221192000
_diffrn_orient_matrix_UB_12      0.0568999000
_diffrn_orient_matrix_UB_13      -0.0927173000
_diffrn_orient_matrix_UB_21      -0.1078017000
_diffrn_orient_matrix_UB_22      -0.0838078000
_diffrn_orient_matrix_UB_23      -0.0072931000
_diffrn_orient_matrix_UB_31      -0.0617130000
_diffrn_orient_matrix_UB_32      0.1254583000
_diffrn_orient_matrix_UB_33      0.0372508000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5966
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.988
_diffrn_reflns_theta_min         4.528
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.194
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile'
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.146
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         5966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0263
_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^)+(0.0455P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0617
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5461
_reflns_number_total             5966
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9987\% 
 around [1.00 0.00 -0.05] (reciprocal) or [1.00 0.00 0.00] (direct)
;
_cod_data_source_file            d1dt01741a2.cif
_cod_data_source_block           tBuPONNOPAg2Cl2
_cod_depositor_comments
'Adding full bibliography for 7707971--7707976.cif.'
_cod_original_cell_volume        1795.44(8)
_cod_database_code               7707973
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C24H40N2O2P2Ag2Cl2
_chemical_oxdiff_usercomment     'MeCN minus 20C'
_olex2_refinement_description
;
1. Others
 Fixed Sof: C4A(0.5) C8A(0.5)
 Fixed U12: C4A(0) C8A(0)
 Fixed U23: C4A(0) C8A(0)
 Fixed Uiso: H3(0.028) H4(0.032) H10A(0.071) H10B(0.071) H10C(0.071)
 H1A(0.057) H1B(0.057) H1C(0.057) H15A(0.066) H15B(0.066) H15C(0.066)
 H14A(0.063) H14B(0.063) H14C(0.063) H11A(0.066) H11B(0.066) H11C(0.066)
 H12A(0.073) H12B(0.073) H12C(0.073) H16A(0.111) H16B(0.111) H16C(0.111)
 Fixed X: H3(0.244349) C4A(0.25) C8A(0.25) H4(0.246054) H10A(0.044731) H10B(-
 0.025428) H10C(0.049452) H1A(0.383398) H1B(0.46974) H1C(0.344364)
 H15A(0.479708) H15B(0.552237) H15C(0.470014) H14A(0.355603) H14B(0.480779)
 H14C(0.397696) H11A(0.133018) H11B(0.061003) H11C(0.188799) H12A(0.190283)
 H12B(0.063793) H12C(0.14612) H16A(0.978299) H16B(0.917951) H16C(0.992743)
 Fixed Y: H3(0.327811) H4(0.197495) H10A(0.642289) H10B(0.773067)
 H10C(0.778485) H1A(0.554043) H1B(0.642296) H1C(0.661064) H15A(0.802655)
 H15B(0.731723) H15C(0.641456) H14A(0.91565) H14B(0.909315) H14C(0.973213)
 H11A(0.997184) H11B(0.981378) H11C(0.99219) H12A(0.771231) H12B(0.747866)
 H12C(0.631968) H16A(0.57236) H16B(0.651439) H16C(0.734416)
 Fixed Z: H3(0.539965) C4A(0.75) C8A(0.75) H4(0.666731) H10A(0.498105)
 H10B(0.469612) H10C(0.554871) H1A(0.40865) H1B(0.359793) H1C(0.336619)
 H15A(0.566424) H15B(0.497291) H15C(0.549088) H14A(0.364284) H14B(0.391118)
 H14C(0.455073) H11A(0.494158) H11B(0.407919) H11C(0.40435) H12A(0.319526)
 H12B(0.325508) H12C(0.358831) H16A(0.718451) H16B(0.791716) H16C(0.72944)
;
_shelx_res_checksum              14751
_shelx_hkl_checksum              40861
_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 1.450
_oxdiff_exptl_absorpt_empirical_full_min 0.754
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2