Construction of modular Pd/Cu multimetallic chains via ligand- and anion-controlled metal-metal interactions
Rivada Wheelaghan, Orestes; Deolka, Shubham; Govindarajan, Ramadoss; Khaskin, Eugene; Fayzullin, Robert R.; Pal, Shrinwantu; Khusnutdinova, Julia R.; Chemical Communications  (2021) –; doi:10.1039/D1CC04212B

data_7128926
_publ_section_title
;
 Construction of modular Pd/Cu multimetallic chains via ligand- and
 anion-controlled metal-metal interactions
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC04212B
_journal_year                    2021
_chemical_formula_moiety
'C28 H29 N3 O P Pd 1+, C32 H12 B F24 1-, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C61.5 H44 B Cl3 F24 N3 O P Pd'
_chemical_formula_weight         1551.52
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-05-08 deposited with the CCDC.	2021-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                108.0714(9)
_cell_angle_beta                 94.0455(8)
_cell_angle_gamma                112.8323(10)
_cell_formula_units_Z            2
_cell_length_a                   13.38647(13)
_cell_length_b                   14.66903(16)
_cell_length_c                   18.73570(19)
_cell_measurement_reflns_used    103806
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      33.1930
_cell_measurement_theta_min      2.3100
_cell_volume                     3146.07(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics
;
WinGX (Farrugia, 2012); Olex2 (Dolomanov et al., 2009);
ORTEP-3 (Farrugia, 2012); PLATON (Spek, 2009)
;
_computing_publication_material
;
WinGX (Farrugia, 2012); Olex2 (Dolomanov et al., 2009);
ORTEP-3 (Farrugia, 2012); PLATON (Spek, 2009); enCIFer (Allen, 2004)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual offset/far'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            254932
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.000
_diffrn_reflns_theta_min         2.258
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.316
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018).
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model. Empirical absorption correction using
spherical harmonics, frame scaling and detector area scaling,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_description       prism
_exptl_crystal_F_000             1550
_exptl_crystal_recrystallization_method
'layering in a DCM/hexane system at r.t.'
_exptl_crystal_size_max          0.302
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.158
_refine_diff_density_max         1.530
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     967
_refine_ls_number_reflns         20078
_refine_ls_number_restraints     245
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0354P)^2^+6.2135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1274
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16247
_reflns_number_total             20078
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04212b2.cif
_cod_data_source_block           jk541
_cod_original_cell_volume        3146.06(6)
_cod_original_formula_sum        'C61.50 H44 B Cl3 F24 N3 O P Pd'
_cod_database_code               7128926
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.848
_shelx_estimated_absorpt_t_max   0.916
_shelx_res_checksum              56949
_shelx_hkl_checksum              26502