Developing five-membered heterocycle substituted phosphinous acids as ligands for palladium-catalyzed Suzuki-Miyaura and Catellani reactions.
Chang, Ting-Wei; Ho, Pei-Yun; Mao, Kuo-Chung; Hong, Fung-E; Dalton transactions (Cambridge, England : 2003) 44 (2015) 17129–17142; doi:10.1039/c5dt02611c

data_7036356
_publ_section_title
;
 Developing five-membered heterocycle substituted phosphinous acids as
 ligands for palladium-catalyzed Suzuki-Miyaura and Catellani reactions.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17129
_journal_page_last               17142
_journal_paper_doi               10.1039/c5dt02611c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C64 H70 Br2 N4 O4 P4 Pd2 S4'
_chemical_formula_sum            'C64 H70 Br2 N4 O4 P4 Pd2 S4'
_chemical_formula_weight         1583.98
_space_group_IT_number           14
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_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
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_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-05-27 deposited with the CCDC.
2015-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 105.090(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.9948(9)
_cell_length_b                   32.593(2)
_cell_length_c                   8.0889(4)
_cell_measurement_reflns_used    3196
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.1360
_cell_measurement_theta_min      3.1980
_cell_volume                     3307.8(4)
_computing_cell_refinement
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CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) 
(compiled Jun 10 2008,16:49:55) 
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_computing_data_collection
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CrysAlis CCD, Oxford Diffraction Ltd., 
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) 
(compiled Jun 10 2008,16:49:55) 
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_computing_data_reduction
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CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) 
(compiled Jun 10 2008,16:49:55) 
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_computing_molecular_graphics    'Bruker SHELXTL'
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_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.863
_diffrn_measurement_device_type  'CCD detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0619
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_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       40
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_diffrn_reflns_limit_l_max       10
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_diffrn_reflns_number            16601
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.13
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_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.024
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_exptl_absorpt_correction_T_min  0.81043
_exptl_absorpt_correction_type   multi-scan
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CrysAlisPro, Agilent Technologies, 
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) 
(compiled Dec  3 2012,18:21:49) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.079
_refine_diff_density_min         -2.376
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.335
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         7677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.335
_refine_ls_R_factor_all          0.1914
_refine_ls_R_factor_gt           0.1621
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+153.8935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3286
_refine_ls_wR_factor_ref         0.3409
_reflns_number_gt                5663
_reflns_number_total             7677
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt02611c2.cif
_cod_data_source_block           ctw05
_cod_depositor_comments
'Adding full bibliography for 7036349--7036358.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7036356