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_7128932
_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
'C82 H72 N8 O2 P2 Pd4 2+, 2(C24 H20 B 1-), 2(C6 H12), 5(C4 H8 O)'
_chemical_formula_sum            'C162 H176 B2 N8 O7 P2 Pd4'
_chemical_formula_weight         2856.26
_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   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-06-01 deposited with the CCDC.	2021-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                72.6084(8)
_cell_angle_beta                 86.4096(6)
_cell_angle_gamma                71.5611(8)
_cell_formula_units_Z            2
_cell_length_a                   14.63077(10)
_cell_length_b                   18.4543(2)
_cell_length_c                   27.6768(2)
_cell_measurement_reflns_used    93235
_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      79.5150
_cell_measurement_theta_min      2.6670
_cell_volume                     6760.82(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics
;
WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012);
PLATON (Spek, 2009); Olex2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
WinGX (Farrugia, 2012); PLATON (Spek, 2009);
Olex2 (Dolomanov et al., 2009); enCIFer (Allen, 2004)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      95(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Rigaku XtaLAB Pro: Kappa dual offset/far'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            136477
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.893
_diffrn_reflns_theta_min         2.641
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.935
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.485
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020).
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            yellow
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       prism
_exptl_crystal_F_000             2968
_exptl_crystal_recrystallization_method
'slow evaporation of a THF/cyclohexane solution at r.t.'
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.068
_refine_diff_density_max         1.652
_refine_diff_density_min         -1.420
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1812
_refine_ls_number_reflns         28766
_refine_ls_number_restraints     992
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0702P)^2^+17.0137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1380
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27281
_reflns_number_total             28766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04212b2.cif
_cod_data_source_block           jk935
_cod_original_cell_volume        6760.85(11)
_cod_database_code               7128932
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.443
_shelx_estimated_absorpt_t_max   0.730
_shelx_res_checksum              60736
_shelx_hkl_checksum              63790