[Di(1-adamantyl)](aryl)phosphine ligands: synthesis, palladium complexation, and catalytic activity.
Sivarajan, Chinraj; Mitra, Raja; Dalton transactions (Cambridge, England : 2003) 54 (2025) 17073–17077; doi:10.1039/d5dt02523k

data_7719800
_publ_section_title
;
 [Di(1-adamantyl)](aryl)phosphine ligands: synthesis, palladium
 complexation, and catalytic activity.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17073
_journal_page_last               17077
_journal_paper_doi               10.1039/d5dt02523k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C29 H36 N P'
_chemical_formula_sum            'C29 H36 N P'
_chemical_formula_weight         429.590
_chemical_name_systematic        CS-SB-005
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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'
_symmetry_Int_Tables_number      14
_audit_creation_date             2025-07-03
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-07-03 deposited with the CCDC.	2025-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.038(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.7324(4)
_cell_length_b                   19.1441(15)
_cell_length_c                   17.393(1)
_cell_measurement_reflns_used    1550
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      25.5030
_cell_measurement_theta_min      2.2240
_cell_volume                     2241.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_collection
'PROGRAM:BIS V6.2.16/2021-10-22 && APEX4 2021.4-0                                '
_computing_data_reduction        'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9577
_diffrn_measured_fraction_theta_max 0.7973
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f    -25.75 154.25   1.00    2.00 -25.75   0.00  73.76    --   180
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0493706000
_diffrn_orient_matrix_UB_12      0.0325259000
_diffrn_orient_matrix_UB_13      0.0029129000
_diffrn_orient_matrix_UB_21      0.0198625000
_diffrn_orient_matrix_UB_22      0.0070485000
_diffrn_orient_matrix_UB_23      -0.0392149000
_diffrn_orient_matrix_UB_31      -0.0908817000
_diffrn_orient_matrix_UB_32      -0.0162492000
_diffrn_orient_matrix_UB_33      -0.0109734000
_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  0.1172
_diffrn_reflns_av_unetI/netI     0.1234
_diffrn_reflns_Laue_measured_fraction_full 0.9577
_diffrn_reflns_Laue_measured_fraction_max 0.7973
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13770
_diffrn_reflns_point_group_measured_fraction_full 0.9577
_diffrn_reflns_point_group_measured_fraction_max 0.7973
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         29.17
_diffrn_reflns_theta_min         1.58
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36319
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.105a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_description       block
_exptl_crystal_F_000             928.843
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.5997
_refine_diff_density_min         -0.7973
_refine_diff_density_rms         0.1581
_refine_ls_d_res_high            0.7291
_refine_ls_d_res_low             12.8722
_refine_ls_goodness_of_fit_ref   1.0140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    60
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4834
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0140
_refine_ls_R_factor_all          0.1325
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          -0.0004
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1103P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1815
_refine_ls_wR_factor_ref         0.2259
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              7
_reflns_limit_h_min              -9
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              -6
_reflns_number_gt                2970
_reflns_number_total             4834
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5dt02523k2.cif
_cod_data_source_block           fastscan_autored
_cod_depositor_comments
'Adding full bibliography for 7719798--7719801.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7719800
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C013(H013), C016(H016), C021(H021), C025(H025), C028(H028), C031(H031)
2.b Secondary CH2 refined with riding coordinates:
 C007(H00a,H00b), C008(H00c,H00d), C009(H00e,H00f), C011(H01a,H01b), C019(H01c,
 H01d), C020(H02a,H02b), C023(H02c,H02d), C024(H02e,H02f), C026(H02g,H02h),
 C027(H02i,H02j), C029(H02k,H02l), C030(H03a,H03b)
2.c Aromatic/amide H refined with riding coordinates:
 C004(H004), C005(H005), C012(H012), C014(H014), C017(H017), C022(H022)
;
_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 1.743
_oxdiff_exptl_absorpt_empirical_full_min 0.619