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_7128928
_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 H28 Cl Cu N3 O P Pd, 2.5(C H2 Cl2)'
_chemical_formula_sum            'C30.5 H33 Cl6 Cu N3 O P Pd'
_chemical_formula_weight         871.21
_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
_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                 108.286(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.5675(4)
_cell_length_b                   16.21405(19)
_cell_length_c                   21.6642(4)
_cell_measurement_reflns_used    43481
_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      70.2730
_cell_measurement_theta_min      3.4320
_cell_volume                     6859.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0895
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            68466
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.248
_diffrn_reflns_theta_min         3.471
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    9.980
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.021
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019).
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    1.687
_exptl_crystal_description       prism
_exptl_crystal_F_000             3496
_exptl_crystal_recrystallization_method
'vapor diffusion in a DCM/hexane system at -30 \%C'
_exptl_crystal_size_max          0.593
_exptl_crystal_size_mid          0.301
_exptl_crystal_size_min          0.197
_refine_diff_density_max         3.828
_refine_diff_density_min         -1.613
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         12362
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0810
_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^)+(0.1418P)^2^+49.7916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2324
_refine_ls_wR_factor_ref         0.2378
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11291
_reflns_number_total             12362
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04212b2.cif
_cod_data_source_block           jk821a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C30.50 H33 Cl6 Cu N3 O P Pd'
_cod_database_code               7128928
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.067
_shelx_estimated_absorpt_t_max   0.244
_shelx_res_checksum              93936
_shelx_hkl_checksum              11040