Neutral, cationic and anionic organonickel and -palladium complexes supported by iminophosphine/phosphinoenaminato ligands.
Santiago, Tomás G; Urbaneja, Carmen; Álvarez, Eleuterio; Ávila, Elena; Palma, Pilar; Cámpora, Juan; Dalton transactions (Cambridge, England : 2003) 49 (2020) 322–335; doi:10.1039/c9dt04062e

data_7701993
_publ_section_title
;
 Neutral, cationic and anionic organonickel and -palladium complexes
 supported by iminophosphine/phosphinoenaminato ligands.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              322
_journal_page_last               335
_journal_paper_doi               10.1039/c9dt04062e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C42 H60 N O2 P Pd Si2'
_chemical_formula_sum            'C42 H60 N O2 P Pd Si2'
_chemical_formula_weight         804.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-11-19 deposited with the CCDC.	2019-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.384(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8081(15)
_cell_length_b                   22.863(3)
_cell_length_c                   14.9029(18)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.85
_cell_measurement_theta_min      2.25
_cell_volume                     4317.4(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.2
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type
; 
 Bruker-Nonius X8kappa APEX II CCD area detector 
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0787
_diffrn_reflns_av_unetI/netI     0.0640
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            62440
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.658
_diffrn_reflns_theta_min         1.643
_exptl_absorpt_coefficient_mu    0.555
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
program SADABS, Bruker (2001). 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       plate
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         3.127
_refine_diff_density_min         -3.406
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         12943
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1306
_refine_ls_R_factor_gt           0.0951
_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^)+(0.1040P)^2^+38.2542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2490
_refine_ls_wR_factor_ref         0.2801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9222
_reflns_number_total             12943
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04062e2.cif
_cod_data_source_block           4c
_cod_depositor_comments
'Adding full bibliography for 7701989--7701993.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7701993
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.897
_shelx_estimated_absorpt_t_max   0.973
_shelx_res_checksum              95566
_shelx_fab_checksum              69800