Comparative study of CO<sub>2</sub> insertion into pincer supported palladium alkyl and aryl complexes.
Deziel, Anthony P.; Gahlawat, Sahil; Hazari, Nilay; Hopmann, Kathrin H.; Mercado, Brandon Q.; Chemical science 14 (2023) 8164–8179; doi:10.1039/d3sc01459b

data_1569514
_publ_section_title
;
 Comparative study of CO<sub>2</sub> insertion into pincer supported
 palladium alkyl and aryl complexes.
;
_journal_issue                   30
_journal_name_full               'Chemical science'
_journal_page_first              8164
_journal_page_last               8179
_journal_paper_doi               10.1039/d3sc01459b
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C31 H51 B N2 P2 Pd'
_chemical_formula_sum            'C31 H51 B N2 P2 Pd'
_chemical_formula_weight         630.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     SHELXT
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-02-20
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-02-21 deposited with the CCDC.	2023-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.790(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9206(9)
_cell_length_b                   17.1954(13)
_cell_length_c                   14.8970(10)
_cell_measurement_reflns_used    4823
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      29.3000
_cell_measurement_theta_min      1.8600
_cell_volume                     3214.3(4)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.965
_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     15.00  64.00   0.50  116.75    --   20.00  54.00-180.00   98
  2  \w    -74.00 108.00   0.50  116.75    --   20.00  54.00-120.00  364
  3  \w    -74.00 -21.00   0.50  116.75    --   20.00  54.00  90.00  106
  4  \w      2.00  27.00   0.50  116.75    --   20.00  54.00  90.00   50
  5  \w    -55.00 -30.00   0.50  116.75    --   20.00  54.00-150.00   50
  6  \w     13.00  61.00   0.50  116.75    --   20.00  54.00-150.00   96
  7  \w     27.00  52.00   0.50  116.75    --   20.00  54.00  60.00   50
  8  \w    -66.00 -11.00   0.50  116.75    --   20.00  54.00 150.00  110
  9  \w    -15.00  10.00   0.50  116.75    --   20.00  54.00-180.00   50
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0247692000
_diffrn_orient_matrix_UB_12      0.0274050000
_diffrn_orient_matrix_UB_13      -0.0237236000
_diffrn_orient_matrix_UB_21      -0.0441573000
_diffrn_orient_matrix_UB_22      -0.0020861000
_diffrn_orient_matrix_UB_23      -0.0387870000
_diffrn_orient_matrix_UB_31      -0.0250927000
_diffrn_orient_matrix_UB_32      0.0307615000
_diffrn_orient_matrix_UB_33      0.0184097000
_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  0.0667
_diffrn_reflns_av_unetI/netI     0.1022
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18745
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.840
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.699
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (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    1.304
_exptl_crystal_description       plate
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         6351
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0277P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0871
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4297
_reflns_number_total             6351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01459b3.cif
_cod_data_source_block           mini2-22007
_cod_depositor_comments
'Adding full bibliography for 1569513--1569521.cif.'
_cod_database_code               1569514
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C31 H51 N2 B P2 Pd'
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.845
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C16(H16A,H16B), C23(H23A,H23B)
1.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C18(H18), C19(H19), C20(H20), C21(H21)
1.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C)
;
_shelx_res_checksum              17327
_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 1.465
_oxdiff_exptl_absorpt_empirical_full_min 0.835