Palladium iminophosphorane complexes: the pre-cursors to the missing link in triphenylphosphane chalcogenide metallacycles.
Fernández-Figueiras, Adolfo; Lucio-Martínez, Fátima; Munín-Cruz, Paula; Polo-Ces, Paula; Reigosa, Francisco; Adams, Harry; Pereira, M. Teresa; Vila, José M; Dalton transactions (Cambridge, England : 2003) 47 (2018) 15801–15807; doi:10.1039/c8dt03062f

data_7047844
_publ_section_title
;
 Palladium iminophosphorane complexes: the pre-cursors to the missing link
 in triphenylphosphane chalcogenide metallacycles.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15801
_journal_page_last               15807
_journal_paper_doi               10.1039/c8dt03062f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C43.5 H36 N O1.5 P2 Pd'
_chemical_formula_weight         765.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2018-07-13 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.266(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
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_cell_length_b                   9.4520(4)
_cell_length_c                   42.7751(14)
_cell_measurement_reflns_used    1987
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.185
_cell_measurement_theta_min      2.315
_cell_volume                     7112.7(5)
_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-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
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_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            48007
_diffrn_reflns_point_group_measured_fraction_full 1.000
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.357
_diffrn_reflns_theta_min         0.962
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_exptl_absorpt_correction_T_max  0.8879
_exptl_absorpt_correction_T_min  0.8095
_exptl_absorpt_correction_type   multi-scans
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3136
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_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.489
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_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         8896
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.748
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0006P)^2^+153.3228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0930
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7841
_reflns_number_total             8896
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03062f2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7047843--7047847.cif.'
_cod_original_formula_sum        'C43.50 H36 N O1.50 P2 Pd'
_cod_database_code               7047844
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.829
_shelx_estimated_absorpt_t_max   0.898
_shelx_res_checksum              69837