Synthesis of pyrrole-based PSiP pincer ligands and their palladium, rhodium, and platinum complexes
Vidlak, Julia F.; Cosio, Mario N.; Sriramaneni, Nihal K.; Bhuvanesh, Nattamai; Ozerov, Oleg V.; Johnson, Miles W.; Dalton Transactions  (2022) –; doi:10.1039/D2DT00948J

data_7710243
_publ_section_title
;
 Synthesis of pyrrole-based PSiP pincer ligands and their palladium,
 rhodium, and platinum complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00948J
_journal_year                    2022
_chemical_formula_moiety         'C33 H29 Cl N2 P2 Pd Si'
_chemical_formula_sum            'C33 H29 Cl N2 P2 Pd Si'
_chemical_formula_weight         685.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-01-21 deposited with the CCDC.	2022-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.8380(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6594(3)
_cell_length_b                   13.5514(4)
_cell_length_c                   23.5488(6)
_cell_measurement_reflns_used    9191
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      30.459
_cell_measurement_theta_min      2.606
_cell_volume                     3053.70(15)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker QUEST PHOTON-III'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            93214
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         1.738
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.865
_exptl_absorpt_correction_T_max  0.3368
_exptl_absorpt_correction_T_min  0.2480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1780 before and 0.0834 after correction.
The Ratio of minimum to maximum transmission is 0.7357.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.478
_exptl_crystal_size_mid          0.452
_exptl_crystal_size_min          0.207
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         7031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0104P)^2^+3.5149P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0502
_refine_ls_wR_factor_ref         0.0524
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6120
_reflns_number_total             7031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00948j2.cif
_cod_data_source_block           nksi43
_cod_database_code               7710243
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.841
_shelx_estimated_absorpt_t_min   0.683
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C4(H4), C29(H29), C2(H2), C15(H15), C3(H3), C33(H33), C8(H8),
 C6(H6), C24(H24), C19(H19), C18(H18), C30(H30), C27(H27), C7(H7), C26(H26),
 C17(H17), C11(H11), C25(H25), C14(H14), C21(H21), C13(H13), C31(H31), C20(H20),
  C32(H32), C12(H12)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_shelx_res_checksum              1382
_olex2_submission_special_instructions 'No special instructions were received'