Palladium(II) Complexes of Bis(diphosphene) with the Different Coordination Behavior
Ura, Rikako; Tsurusaki, Akihiro; Kamikawa, Ken; Dalton Transactions  (2022) –; doi:10.1039/D1DT03806K

data_7709305
_publ_section_title
;
 Palladium(II) Complexes of Bis(diphosphene) with the Different
 Coordination Behavior
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03806K
_journal_year                    2022
_chemical_formula_moiety         'C78 H86 P4, 2(C7 H8)'
_chemical_formula_sum            'C92 H102 P4'
_chemical_formula_weight         1331.61
_chemical_melting_point          153
_chemical_name_systematic
1,2-bis(2-(2,4-6-tri-tert-butylphenyl)diphosphenyl)-[1,1'-binaphthalen]-3-yl)ethane
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-11-10 deposited with the CCDC.	2022-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                101.884(4)
_cell_angle_beta                 96.491(2)
_cell_angle_gamma                105.675(2)
_cell_formula_units_Z            1
_cell_length_a                   10.603(4)
_cell_length_b                   13.870(5)
_cell_length_c                   13.974(5)
_cell_measurement_reflns_used    5694
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      27.4700
_cell_measurement_theta_min      3.0484
_cell_volume                     1904.9(12)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    '<i>ORTEP-3</i> (Farrugia, 1997)'
_computing_publication_material
'<i>SHELXL-2014/7</i> and <i>Yadokari-XG 2009</i> (Kabuto <i>et al.</i>, 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2014 (Giacovazzo <i>et al.</i>, 2015)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19605
_diffrn_reflns_point_group_measured_fraction_full 0.884
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         3.048
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9313
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_description       Prism
_exptl_crystal_F_000             714
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene/hexane'
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 4700 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         14949
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0574P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0966
_reflns_Friedel_coverage         0.742
_reflns_Friedel_fraction_full    0.778
_reflns_Friedel_fraction_max     0.728
_reflns_number_gt                12784
_reflns_number_total             14949
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03806k2.cif
_cod_data_source_block           SS-2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        1904.9(11)
_cod_database_code               7709305
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.962
_shelx_estimated_absorpt_t_max   0.976
_shelx_res_checksum              44338
_shelx_hkl_checksum              36226