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_7035438
_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         '2(C42 H34 N6 O2 P2), C2 H3 N'
_chemical_formula_sum            'C86 H71 N13 O4 P4'
_chemical_formula_weight         1474.44
_space_group_IT_number           14
_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   geom
_atom_sites_solution_primary     direct
_audit_update_record
;
2014-10-31 deposited with the CCDC.
2015-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.6830(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.8008(2)
_cell_length_b                   16.6628(3)
_cell_length_c                   17.8668(3)
_cell_measurement_reflns_used    31838
_cell_measurement_temperature    175
_cell_measurement_theta_max      28.9856
_cell_measurement_theta_min      2.8568
_cell_volume                     3756.65(11)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_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 8.4205
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_details
;
  1 omega    3.00  101.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4101   77.0000  120.0000 98

  2 omega  -14.00  101.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4101   77.0000 -120.0000 115

  3 omega  -19.00   85.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4101   77.0000   30.0000 104

  4 omega  -57.00   69.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.5351   77.0000  120.0000 126

  5 omega  -61.00   50.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.5351   77.0000    0.0000 111

  6 omega  -61.00   50.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.5351   77.0000 -120.0000 111

  7 omega   34.00  118.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4101  179.0000   30.0000 84

  8 omega  -59.00  -24.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.5351   38.0000   90.0000 35

  9 omega  -59.00   67.00   1.0000   22.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.5351   38.0000 -150.0000 126

;
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0124929000
_diffrn_orient_matrix_UB_12      0.0381873000
_diffrn_orient_matrix_UB_13      -0.0166372000
_diffrn_orient_matrix_UB_21      0.0259241000
_diffrn_orient_matrix_UB_22      -0.0105436000
_diffrn_orient_matrix_UB_23      -0.0307026000
_diffrn_orient_matrix_UB_31      -0.0483052000
_diffrn_orient_matrix_UB_32      -0.0155360000
_diffrn_orient_matrix_UB_33      -0.0200684000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_av_sigmaI/netI    0.0559
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            64742
_diffrn_reflns_theta_full        26.726
_diffrn_reflns_theta_max         29.050
_diffrn_reflns_theta_min         2.863
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.49
_refine_diff_density_min         -0.67
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8507
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         9225
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.0008743
_refine_ls_shift/su_mean         0.0000359
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.10P)^2^ + 3.94P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1425
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1425
_reflns_limit_h_max              16
_reflns_limit_h_min              -17
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                7926
_reflns_number_total             9225
_reflns_threshold_expression     I>2.0\s(I)
_oxford_refine_ls_scale          3.16(3)
_cod_data_source_file            c5dt02197a2.cif
_cod_data_source_block           8.1
_cod_depositor_comments
'Adding full bibliography for 7035438--7035443.cif.'
_cod_original_cell_volume        3756.64(11)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               7035438
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE P(1,X'S, U'S) UNTIL C(20) 
CONT  C(21,X'S, U'S) UNTIL C(26) 
CONT  C(27,X'S, U'S) UNTIL C(33) 
CONT  C(34,X'S, U'S) UNTIL C(40) 
CONT  C(41,X'S, U'S) UNTIL C(46) 
CONT  C(47,X'S, U'S) UNTIL C(52) 
CONT  C(53,X'S) UNTIL N(54) 
EQUIV C(53,U[ISO]) N(54,U[ISO]) 
RIDE C   (  16,X'S) H   ( 161,X'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   (  22,X'S) H   ( 221,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   ( 272,X'S) H   ( 271,X'S) 
RIDE C   (  29,X'S) H   ( 291,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   ( 342,X'S) H   ( 341,X'S) 
RIDE C   (  36,X'S) H   ( 361,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   (  42,X'S) H   ( 421,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   (  48,X'S) H   ( 481,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) H   ( 532,X'S) H   ( 533,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
DIST  1.08 , .01 =      C(53) TO N(54) 
DIST  1.47 , .01 =      C(53) TO C(53,-1,1,1,1) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;