Double [3 + 2]-dimerisation cascade synthesis of bis(triazolyl)bisphosphanes, a new scaffold for bidentate bisphosphanes.
Laborde, Coralie; Wei, Muh-Mei; van der Lee, Arie; Deydier, Eric; Daran, Jean-Claude; Volle, Jean-Noël; Poli, Rinaldo; Pirat, Jean-Luc; Manoury, Eric; Virieux, David; Dalton transactions (Cambridge, England : 2003) 44 (2015) 12539–12545; doi:10.1039/c5dt02197a

data_7035441
_publ_section_title
;
 Double [3 + 2]-dimerisation cascade synthesis of
 bis(triazolyl)bisphosphanes, a new scaffold for bidentate bisphosphanes.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12539
_journal_page_last               12545
_journal_paper_doi               10.1039/c5dt02197a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C42 H34 Cl2 N6 P2 Pd, 4(C2 H3 N)'
_chemical_formula_sum            'C50 H46 Cl2 N10 P2 Pd'
_chemical_formula_weight         1026.21
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2014-10-31 deposited with the CCDC.
2015-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.5985(2)
_cell_length_b                   10.81823(12)
_cell_length_c                   20.4451(3)
_cell_measurement_reflns_used    14336
_cell_measurement_temperature    175
_cell_measurement_theta_max      67.4550
_cell_measurement_theta_min      2.1590
_cell_volume                     4998.33(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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      175
_diffrn_detector_area_resol_mean 16.0143
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
  1 omega -106.00  -40.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.6428 -179.0000 -150.0000 66

  2 omega -102.00  -13.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.6428  -57.0000  120.0000 89

  3 omega  -45.00    5.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.6428   57.0000   60.0000 50

  4 omega  -45.00  -17.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000 -120.0000 28

  5 omega -113.00  -87.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000 -140.0000   48.0000 26

  6 omega   39.00   91.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -25.0000  150.0000 52

  7 omega  126.00  172.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   25.0000  150.0000 46

  8 omega   50.00   76.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -50.0000 -180.0000 26

  9 omega   78.00  142.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   64.0000 -120.0000 64

 10 omega   93.00  119.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  179.0000  -60.0000 26

 11 omega   49.00  103.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000 -112.0000 -180.0000 54

 12 omega   74.00  108.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   25.0000  150.0000 34

 13 omega  108.00  134.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  112.0000  150.0000 26

 14 omega  106.00  157.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  112.0000  120.0000 51

 15 omega   78.00  149.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   64.0000  -60.0000 71

 16 omega   33.00  109.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -64.0000 -180.0000 76

 17 omega   45.00   87.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -50.0000 -150.0000 42

 18 omega   64.00   90.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  179.0000  -60.0000 26

 19 omega  101.00  158.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  112.0000  -60.0000 57

 20 omega   34.00   92.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -38.0000  -60.0000 58

 21 omega   91.00  116.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000 -112.0000 -150.0000 25

 22 omega  144.00  170.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   50.0000  -30.0000 26

 23 omega   96.00  128.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   50.0000  -30.0000 32

 24 omega  -55.00   35.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.6428   57.0000  -90.0000 90

 25 omega   -4.00   76.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       33.6428  -99.0000  120.0000 80

 26 omega   13.00  102.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       33.6428   57.0000  -90.0000 89

 27 omega   13.00  102.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -       33.6428   57.0000   30.0000 89

 28 omega   74.00  172.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   38.0000   90.0000 98

 29 omega   28.00  116.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000 -112.0000    0.0000 88

 30 omega   30.00  104.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -50.0000    0.0000 74

 31 omega   74.00  172.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   38.0000   30.0000 98

 32 omega   70.00  170.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   77.0000  -90.0000 100

 33 omega   74.00  172.00   1.0000   13.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   38.0000 -150.0000 98

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0604893000
_diffrn_orient_matrix_UB_12      0.0305777000
_diffrn_orient_matrix_UB_13      0.0308878000
_diffrn_orient_matrix_UB_21      0.0142212000
_diffrn_orient_matrix_UB_22      -0.1390091000
_diffrn_orient_matrix_UB_23      0.0045932000
_diffrn_orient_matrix_UB_31      0.0280727000
_diffrn_orient_matrix_UB_32      0.0044655000
_diffrn_orient_matrix_UB_33      -0.0685592000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42569
_diffrn_reflns_theta_full        62.764
_diffrn_reflns_theta_max         67.488
_diffrn_reflns_theta_min         3.912
_exptl_absorpt_coefficient_mu    4.937
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
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            'yellow transparent'
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.74
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9571
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         7634
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.0014202
_refine_ls_shift/su_mean         0.0000394
_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: 
 15.5 -22.6 14.2 -8.79 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0494
_refine_ls_wR_factor_gt          0.0408
_refine_ls_wR_factor_ref         0.0408
_reflns_limit_h_max              27
_reflns_limit_h_min              -26
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                7634
_reflns_number_total             8878
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_scale          1.6093(15)
_cod_data_source_file            c5dt02197a2.cif
_cod_data_source_block           13.11
_cod_depositor_comments
'Adding full bibliography for 7035438--7035443.cif.'
_cod_original_cell_volume        4998.32(9)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7035441
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 282,X'S) H   ( 281,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S)
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 352,X'S) H   ( 351,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) H   ( 562,X'S) H   ( 563,X'S) 
RIDE C   (  59,X'S) H   ( 593,X'S) H   ( 592,X'S) H   ( 591,X'S) 
RIDE C   (  62,X'S) H   ( 623,X'S) H   ( 622,X'S) H   ( 621,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) H   ( 652,X'S) H   ( 653,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;