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_7707972
_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 N2 O2 P2'
_chemical_formula_sum            'C24 H40 N2 O2 P2'
_chemical_formula_weight         450.52
_chemical_name_systematic        tBuPONNOP
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_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                83.368(9)
_cell_angle_beta                 87.909(8)
_cell_angle_gamma                77.724(10)
_cell_formula_units_Z            2
_cell_length_a                   6.3190(7)
_cell_length_b                   14.4208(18)
_cell_length_c                   15.1492(15)
_cell_measurement_reflns_used    1538
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      70.9590
_cell_measurement_theta_min      13.9760
_cell_volume                     1339.8(3)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.956
_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   -107.00  -6.00   1.00   10.00    --  -35.53 -19.00  90.00  101
  2  \w    -51.00  32.00   1.00   10.00    --  -35.53  57.00 -90.00   83
  3  \w   -103.00 -21.00   1.00   10.00    --  -35.53 -57.00  30.00   82
  4  \w     31.00  87.00   1.00   10.00    --   35.53-125.00-180.00   56
  5  \w      9.00  70.00   1.00   10.00    --   35.53 -99.00 -30.00   61
  6  \w     68.00 113.00   1.00   45.00    --  105.15 -45.00 150.00   45
  7  \w     54.00 115.00   1.00   45.00    --  105.15 -61.00 -30.00   61
  8  \w     88.00 173.00   1.00   45.00    --  105.15  45.00  30.00   85
  9  \w     67.00 106.00   1.00   45.00    --  105.15 -95.00 -30.00   39
 10  \w     51.00 106.00   1.00   45.00    --  105.15 -95.00 -90.00   55
 11  \w     87.00 123.00   1.00   45.00    --  105.15  61.00  60.00   36
 12  \w    140.00 172.00   1.00   45.00    --  105.15  61.00  60.00   32
 13  \w    105.00 175.00   1.00   45.00    --  105.15 111.00 -30.00   70
 14  \w     74.00 109.00   1.00   45.00    --  105.15-111.00-150.00   35
 15  \w     49.00 122.00   1.00   45.00    --  105.15 -45.00-120.00   73
 16  \w     40.00 119.00   1.00   45.00    --  105.15 -45.00  60.00   79
 17  \w     67.00 171.00   1.00   45.00    --  105.15  15.00 150.00  104
 18  \w     56.00 107.00   1.00   45.00    --  105.15 -77.00  60.00   51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8311
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.959
_diffrn_reflns_theta_min         4.068
_exptl_absorpt_coefficient_mu    1.627
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.824
_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    1.117
_exptl_crystal_description       plate
_exptl_crystal_F_000             488
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene/hexane'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.029
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         8311
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0531P)^2^+1.4174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1776
_refine_ls_wR_factor_ref         0.1889
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5380
_reflns_number_total             8311
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9602\% 
around [0.89 0.45 0.00] (reciprocal) or [1.00 0.00 -0.02] (direct)
;
_cod_data_source_file            d1dt01741a2.cif
_cod_data_source_block           tbuponnop
_cod_depositor_comments
'Adding full bibliography for 7707971--7707976.cif.'
_cod_database_code               7707972
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.726
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5189(17)
 0.4811(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C5(H5), C4(H4)
3.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C15(H15A,H15B,
 H15C), C22(H22A,H22B,H22C), C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C23(H23A,
 H23B,H23C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C)
;
_shelx_res_checksum              11797
_shelx_hkl_checksum              16807
_olex2_submission_original_sample_id tBuPONNOP
_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
;