Multifaceted role of silver salts as ligand scavengers and different behavior of nickel and palladium complexes: beyond halide abstraction.
Pérez-Ortega, Ignacio; Albéniz, Ana C; Dalton transactions (Cambridge, England : 2003) 52 (2023) 1425–1432; doi:10.1039/d2dt03948f

data_7712051
_publ_section_title
;
 Multifaceted role of silver salts as ligand scavengers and different
 behavior of nickel and palladium complexes: beyond halide abstraction.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1425
_journal_page_last               1432
_journal_paper_doi               10.1039/d2dt03948f
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C32 H33 F3 Ni O P S, 2(C H Cl3), B F4'
_chemical_formula_sum            'C34 H35 B Cl6 F7 Ni O P S'
_chemical_formula_weight         937.87
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-09-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-11-18 deposited with the CCDC.	2023-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.7171(6)
_cell_length_b                   14.3676(6)
_cell_length_c                   37.0248(11)
_cell_measurement_reflns_used    6618
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.2540
_cell_measurement_theta_min      3.5590
_cell_volume                     8892.8(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.808
_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     29.00  90.00   1.00   34.26    --   12.51  19.00  30.00   61
  2  \w    -21.00  26.00   1.00   34.26    --   12.51  19.00  30.00   47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0067349000
_diffrn_orient_matrix_UB_12      0.0442488000
_diffrn_orient_matrix_UB_13      0.0079399000
_diffrn_orient_matrix_UB_21      0.0216919000
_diffrn_orient_matrix_UB_22      0.0214531000
_diffrn_orient_matrix_UB_23      -0.0142209000
_diffrn_orient_matrix_UB_31      -0.0358143000
_diffrn_orient_matrix_UB_32      0.0046530000
_diffrn_orient_matrix_UB_33      -0.0100844000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.808
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            24643
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.808
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.808
_diffrn_reflns_theta_min         3.267
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.935
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.668
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       block
_exptl_crystal_F_000             3808
_exptl_crystal_size_max          0.524
_exptl_crystal_size_mid          0.524
_exptl_crystal_size_min          0.319
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         10307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1476
_refine_ls_R_factor_gt           0.0896
_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^)+(0.1289P)^2^+13.3833P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2418
_refine_ls_wR_factor_ref         0.2851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5641
_reflns_number_total             10307
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03948f2.cif
_cod_data_source_block           23-10-2019
_cod_depositor_comments
'Adding full bibliography for 7712049--7712051.cif.'
_cod_original_cell_volume        8892.7(5)
_cod_database_code               7712051
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C32 H24 B F7 O P S Ni'
_chemical_oxdiff_usercomment     'Yellow block'
_reflns_odcompleteness_completeness 98.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C32(H32), C33(H33)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10a,H10b)
2.c Aromatic/amide H refined with riding coordinates:
 C31(H31), C27(H27), C23(H23), C30(H30), C22(H22), C19(H19), C28(H28),
 C15(H15), C18(H18), C6(H6), C20(H20), C29(H29), C5(H5), C24(H24), C17(H17),
 C3(H3), C16(H16), C4(H4), C25(H25)
2.d Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C9(H9a,H9b,H9c), C12(H12a,H12b,H12c), C34(H34a,H34b,H34c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              23840
_shelx_hkl_checksum              78185
_shelx_fab_checksum              11394
_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 1.149
_oxdiff_exptl_absorpt_empirical_full_min 0.921