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_7710241
_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         'C32 H28 Cl2 N2 P2 Pt'
_chemical_formula_sum            'C32 H28 Cl2 N2 P2 Pt'
_chemical_formula_weight         768.49
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-11
_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                99.4630(10)
_cell_angle_beta                 100.9600(10)
_cell_angle_gamma                111.2430(10)
_cell_formula_units_Z            2
_cell_length_a                   9.3937(4)
_cell_length_b                   12.2210(4)
_cell_length_c                   14.1646(5)
_cell_measurement_reflns_used    9825
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      27.578
_cell_measurement_theta_min      2.373
_cell_volume                     1438.79(9)
_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 0.994
_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  0.0291
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26811
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.595
_diffrn_reflns_theta_min         1.849
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.199
_exptl_absorpt_correction_T_max  0.3334
_exptl_absorpt_correction_T_min  0.2010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0786 before and 0.0400 after correction.
The Ratio of minimum to maximum transmission is 0.6029.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.081
_refine_diff_density_max         1.560
_refine_diff_density_min         -1.247
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         6631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0244
_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^)+3.7605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0540
_refine_ls_wR_factor_ref         0.0554
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6256
_reflns_number_total             6631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00948j2.cif
_cod_data_source_block           mwjiii4041a
_cod_database_code               7710241
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.678
_shelx_estimated_absorpt_t_min   0.412
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C22(H22),
  C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30),
 C31(H31), C32(H32)
;
_shelx_res_checksum              87557
_olex2_submission_special_instructions 'No special instructions were received'