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_7707974
_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 Au2 Cl2 N2 O2 P2, C H2 Cl2'
_chemical_formula_sum            'C25 H42 Au2 Cl4 N2 O2 P2'
_chemical_formula_weight         1000.28
_chemical_name_systematic        tBuPONNOPAu2Cl2
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-27
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.4412(6)
_cell_length_b                   19.7582(8)
_cell_length_c                   24.0737(11)
_cell_measurement_reflns_used    8948
_cell_measurement_temperature    149.98(11)
_cell_measurement_theta_max      31.8830
_cell_measurement_theta_min      1.8800
_cell_volume                     6869.0(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1872
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.886
_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    -13.00  41.00   1.00   50.00    --   18.00  77.00-120.00   54
  2  \w     49.00  91.00   1.00   50.00    --   18.00 178.00  90.00   42
  3  \w     17.00  67.00   1.00   50.00    --   18.00  19.00 120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0082997000
_diffrn_orient_matrix_UB_12      0.0295488000
_diffrn_orient_matrix_UB_13      0.0159601000
_diffrn_orient_matrix_UB_21      -0.0423594000
_diffrn_orient_matrix_UB_22      0.0051158000
_diffrn_orient_matrix_UB_23      -0.0143389000
_diffrn_orient_matrix_UB_31      -0.0234323000
_diffrn_orient_matrix_UB_32      -0.0197175000
_diffrn_orient_matrix_UB_33      0.0202070000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            29294
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.460
_diffrn_reflns_theta_min         1.692
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.962
_exptl_absorpt_correction_T_max  0.376
_exptl_absorpt_correction_T_min  0.164
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.934
_exptl_crystal_description       plate
_exptl_crystal_F_000             3824
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane/hexane'
_exptl_crystal_size_max          0.344
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.135
_refine_diff_density_max         0.981
_refine_diff_density_min         -1.348
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         10978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0236P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0740
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8118
_reflns_number_total             10978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01741a2.cif
_cod_data_source_block           Au2Cl2tBuPONNOP
_cod_depositor_comments
'Adding full bibliography for 7707971--7707976.cif.'
_cod_database_code               7707974
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Au2Cl2P2N2O2C40H30
_shelx_estimated_absorpt_t_max   0.378
_shelx_estimated_absorpt_t_min   0.149
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.51
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H25A)=Sof(H25B)=Sof(Cl3B)=1-FVAR(1)
 Sof(Cl3A)=Sof(H25C)=Sof(H25D)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C25(H25C,H25D), C25(H25A,H25B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C4(H4)
3.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C21(H21A,H21B,H21C), C13(H13A,H13B,H13C), C20(H20A,H20B,
 H20C), C18(H18A,H18B,H18C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C14(H14A,
 H14B,H14C), C16(H16A,H16B,H16C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C),
 C19(H19A,H19B,H19C)
;
_shelx_res_checksum              57990
_shelx_hkl_checksum              82828
_ins_header
;
TITL AD150_beamstop in Pbca 
REM Pbca (#61 in standard setting)
CELL 0.71073  14.441236  19.758249  24.073651  90.0000  90.0000  90.0000
ZERR    7.00   0.000629   0.000813   0.001137   0.0000   0.0000   0.0000
LATT  1
SYMM -x+1/2,-y, z+1/2 
SYMM -x, y+1/2,-z+1/2 
SYMM  x+1/2,-y+1/2,-z 
SFAC C H N O P Cl Au
UNIT 280.00 210.00 14.00 14.00 14.00 14.00 14.00
REM  CrysAlisPro recorded range (K): Min=149.9; max=150.1; aver:150.0
TEMP -123
SIZE 0.14 0.27 0.34
TREF
HKLF 4
END
;
_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 1.233
_oxdiff_exptl_absorpt_empirical_full_min 0.777