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_7035439
_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         'C36 H38 N6 O2 P2'
_chemical_formula_sum            'C36 H38 N6 O2 P2'
_chemical_formula_weight         648.66
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 90.8818(18)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.4908(5)
_cell_length_b                   11.0856(2)
_cell_length_c                   25.9333(5)
_cell_measurement_reflns_used    10890
_cell_measurement_temperature    175
_cell_measurement_theta_max      28.8960
_cell_measurement_theta_min      1.5890
_cell_volume                     6752.5(2)
_computing_cell_refinement
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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)
;
_computing_data_collection
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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)
;
_computing_data_reduction
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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)
;
_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 0.966
_diffrn_measured_fraction_theta_max 0.878
_diffrn_measurement_details
;
  1 omega  -10.00   71.00   1.0000  170.0000
omega____ theta____ kappa____ phi______ frames
    -       15.4892   77.0000  150.0000 81

  2 omega   -6.00   83.00   1.0000  170.0000
omega____ theta____ kappa____ phi______ frames
    -       15.4892   77.0000  -90.0000 89

  3 omega  -11.00   83.00   1.0000  170.0000
omega____ theta____ kappa____ phi______ frames
    -       15.4892   77.0000   30.0000 94

  4 omega   52.00   82.00   1.0000  170.0000
omega____ theta____ kappa____ phi______ frames
    -       15.4892   77.0000 -180.0000 30

  5 omega  -14.00   47.00   1.0000  170.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2704   77.0000 -150.0000 61

  6 omega   25.00   46.00   1.0000  170.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2704   77.0000  150.0000 21

;
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0245429000
_diffrn_orient_matrix_UB_12      0.0199455000
_diffrn_orient_matrix_UB_13      -0.0131162000
_diffrn_orient_matrix_UB_21      -0.0033961000
_diffrn_orient_matrix_UB_22      0.0584174000
_diffrn_orient_matrix_UB_23      0.0106869000
_diffrn_orient_matrix_UB_31      0.0172527000
_diffrn_orient_matrix_UB_32      -0.0168612000
_diffrn_orient_matrix_UB_33      0.0214986000
_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  0.047
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            27328
_diffrn_reflns_theta_full        25.190
_diffrn_reflns_theta_max         29.290
_diffrn_reflns_theta_min         1.571
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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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            colourless
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.27
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0885
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6655
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.0020464
_refine_ls_shift/su_mean         0.0000649
_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: 
 8.12 6.38 7.13 2.16 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0602
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0552
_reflns_limit_h_max              30
_reflns_limit_h_min              -31
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                6655
_reflns_number_total             8090
_reflns_threshold_expression     I>2.0\s(I)
_oxford_reflns_number_all        8090
_cod_data_source_file            c5dt02197a2.cif
_cod_data_source_block           8.3
_cod_depositor_comments
'Adding full bibliography for 7035438--7035443.cif.'
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_database_code               7035439
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'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                                                                             
;