Synthesis of a Helical Phosphine and a Catalytic Study of Its Palladium Complex.
Beránek, Tomáš; Žádný, Jaroslav; Strašák, Tomáš; Karban, Jindřich; Císařová, Ivana; Sýkora, Jan; Storch, Jan; ACS omega 5 (2020) 882–892; doi:10.1021/acsomega.9b03830

data_4517297
_publ_section_title
;
 Synthesis of a Helical Phosphine and a Catalytic Study of Its Palladium
 Complex.
;
_journal_issue                   1
_journal_name_full               'ACS omega'
_journal_page_first              882
_journal_page_last               892
_journal_paper_doi               10.1021/acsomega.9b03830
_journal_volume                  5
_journal_year                    2020
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C84 H54 Cl2 P2 Pd'
_chemical_formula_sum            'C84 H54 Cl2 P2 Pd'
_chemical_formula_weight         1302.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 97.375(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6600(10)
_cell_length_b                   15.5656(8)
_cell_length_c                   28.2198(16)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      61.0014
_cell_measurement_theta_min      2.8389
_cell_volume                     7257.5(7)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service vV6.2.4'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Helios Cu  multilayer optic'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1034
_diffrn_reflns_av_unetI/netI     0.1866
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            49610
_diffrn_reflns_point_group_measured_fraction_full 0.927
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        62.723
_diffrn_reflns_theta_max         62.723
_diffrn_reflns_theta_min         2.839
_diffrn_source                   'I\mS  micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.474
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.32
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       prism
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.352
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.086
_refine_diff_density_max         1.461
_refine_diff_density_min         -1.309
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.40(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         21584
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.2117
_refine_ls_R_factor_gt           0.1004
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1709P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2611
_refine_ls_wR_factor_ref         0.3273
_reflns_Friedel_coverage         0.903
_reflns_Friedel_fraction_full    0.880
_reflns_Friedel_fraction_max     0.880
_reflns_number_gt                8921
_reflns_number_total             21584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b03830_si_002.cif
_cod_data_source_block           tb_pdhelix_sykora_sq
_cod_depositor_comments
;
         Adding full bibliography for 4517297.cif.

2020-05-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C168 H108 Cl4 P4 Pd2'
_cod_original_formula_weight         2605.02
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               4517297
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.374
_shelx_estimated_absorpt_t_max   0.754
_shelx_res_checksum              679
_shelx_hkl_checksum              74850
_shelx_fab_checksum              21977