Palladium(ii) pincer complexes of a C,C,C-NHC, diphosphonium bis(ylide) ligand.
Taakili, Rachid; Lepetit, Christine; Duhayon, Carine; Valyaev, Dmitry A.; Lugan, Noël; Canac, Yves; Dalton transactions (Cambridge, England : 2003) 48 (2019) 1709–1721; doi:10.1039/c8dt04316g

data_7048600
_publ_section_title
;
 Palladium(ii) pincer complexes of a C,C,C-NHC, diphosphonium bis(ylide)
 ligand.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1709
_journal_page_last               1721
_journal_paper_doi               10.1039/c8dt04316g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C50 H51 N3 P2 Pd, 2(C F3 O3 S), 0.6(H2 O)'
_chemical_formula_sum            'C52 H52.2 F6 N3 O6.6 P2 Pd S2'
_chemical_formula_weight         1171.27
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2018-12-20 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.366(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6658(9)
_cell_length_b                   17.1283(10)
_cell_length_c                   21.6507(13)
_cell_measurement_reflns_used    7112
_cell_measurement_temperature    100
_cell_measurement_theta_max      21
_cell_measurement_theta_min      3
_cell_volume                     5066.4(5)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.170
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            103825
_diffrn_reflns_theta_full        25.396
_diffrn_reflns_theta_max         25.396
_diffrn_reflns_theta_min         1.516
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.54
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2395.200
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.94
_refine_diff_density_min         -1.73
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1047
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         5636
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.1383
_refine_ls_R_factor_gt           0.0840
_refine_ls_shift/su_max          0.0010463
_refine_ls_shift/su_mean         0.0000247
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.839 0.704 0.507 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1306
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0857
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                5841
_reflns_number_total             9276
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_r_factor_ref   0.0808
_oxford_reflns_number_all        9252
_oxford_reflns_threshold_expression_ref I>2.2\s(I)
_cod_data_source_file            c8dt04316g2.cif
_cod_data_source_block           I_CCDC1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7048596--7048601.cif.
;
_cod_original_sg_symbol_Hall     ' -P 2yn'
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C52 H52.2 F6 N3 O6.60 P2 Pd1 S2'
_cod_database_code               7048600