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_7128927
_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_absolute_configuration ad
_chemical_formula_moiety         'C28 H28 N3 O P Pd, C2 H4 O2, C H2 Cl2'
_chemical_formula_sum            'C31 H34 Cl2 N3 O3 P Pd'
_chemical_formula_weight         704.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 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                90
_cell_angle_beta                 104.0699(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.78647(4)
_cell_length_b                   13.20388(5)
_cell_length_c                   15.31398(7)
_cell_measurement_reflns_used    52822
_cell_measurement_temperature    94(2)
_cell_measurement_theta_max      79.5550
_cell_measurement_theta_min      3.3440
_cell_volume                     1527.221(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.76a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.76a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.76a (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      94(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.979
_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  0.0422
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34807
_diffrn_reflns_point_group_measured_fraction_full 0.921
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.825
_diffrn_reflns_theta_min         4.480
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    7.307
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.420
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.76a (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    1.533
_exptl_crystal_description       prism
_exptl_crystal_F_000             720
_exptl_crystal_recrystallization_method
'vapor diffusion in a DCM/pentane system at -30 \%C'
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.026
_refine_diff_density_max         1.324
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 2624 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         5974
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0532P)^2^+0.9626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0878
_reflns_Friedel_coverage         0.831
_reflns_Friedel_fraction_full    0.850
_reflns_Friedel_fraction_max     0.818
_reflns_number_gt                5919
_reflns_number_total             5974
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04212b2.cif
_cod_data_source_block           jk838
_cod_original_cell_volume        1527.222(12)
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               7128927
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.368
_shelx_estimated_absorpt_t_max   0.833
_shelx_res_checksum              17638
_shelx_hkl_checksum              69867