New 1,2,3-triazole based bis- and trisphosphine ligands: synthesis, transition metal chemistry and catalytic studies.
Radhakrishna, Latchupatula; Kunchur, Harish S.; Namdeo, Pavan K.; Butcher, Ray J.; Balakrishna, Maravanji S.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 3434–3449; doi:10.1039/c9dt04302k

data_7703169
_publ_section_title
;
 New 1,2,3-triazole based bis- and trisphosphine ligands: synthesis,
 transition metal chemistry and catalytic studies.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3434
_journal_page_last               3449
_journal_paper_doi               10.1039/c9dt04302k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C38 H28 Cl N3 Ni P2, 3(C6 H6)'
_chemical_formula_sum            'C56 H46 Cl N3 Ni P2'
_chemical_formula_weight         917.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-25 deposited with the CCDC.	2020-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                87.1739(12)
_cell_angle_beta                 81.6515(12)
_cell_angle_gamma                71.6855(13)
_cell_formula_units_Z            2
_cell_length_a                   10.05434(14)
_cell_length_b                   11.14458(16)
_cell_length_c                   22.0783(3)
_cell_measurement_reflns_used    33716
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.2860
_cell_measurement_theta_min      2.0170
_cell_volume                     2323.69(6)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -110.00  19.00   0.50   16.00    --  -20.00 -72.00-180.00  258
  2  \w   -110.00  16.00   0.50   16.00    --  -20.00   0.00-180.00  252
  3  \w    -79.00  19.00   0.50   16.00    --  -20.00 -72.00 -36.00  196
  4  \w    -58.50 -24.50   0.50   16.00    --  -20.00 -72.00 108.00   68
  5  \w    -34.50   5.00   0.50   16.00    --  -20.00 -72.00  36.00   79
  6  \w    -59.00 -28.50   0.50   16.00    --  -20.00  72.00-180.00   61
  7  \w    -63.00  70.00   0.50   16.00    --  -20.00   0.00  36.00  266
  8  \w   -110.00  19.00   0.50   16.00    --  -20.00 -72.00-108.00  258
  9  \w    -59.00 -23.00   0.50   16.00    --  -20.00  72.00 108.00   72
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.902
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            46256
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.214
_diffrn_reflns_theta_min         2.227
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87597
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.15 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       block
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         13613
_refine_ls_number_restraints     258
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+0.6418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0950
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12000
_reflns_number_total             13613
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04302k2.cif
_cod_data_source_block           compound-17
_cod_depositor_comments
'Adding full bibliography for 7703162--7703172.cif.'
_cod_database_code               7703169
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.877
_shelx_estimated_absorpt_t_min   0.844
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 P1-C15 \\sim P1-C0
 with sigma of 0.02
 C15-C20 \\sim C0-C2AA
 with sigma of 0.02
 C15-C16 \\sim C0-C4BA
 with sigma of 0.02
 C20-C19 \\sim C2AA-C1AA
 with sigma of 0.02
 C16-C17 \\sim C4BA-C0AA
 with sigma of 0.02
 C18-C19 \\sim C5BA-C1AA
 with sigma of 0.02
 C18-C17 \\sim C5BA-C0AA
 with sigma of 0.02
 P1-C20 \\sim P1-C2AA
 with sigma of 0.04
 P1-C16 \\sim P1-C4BA
 with sigma of 0.04
 C15-C19 \\sim C0-C1AA
 with sigma of 0.04
 C15-C17 \\sim C0-C0AA
 with sigma of 0.04
 C20-C16 \\sim C2AA-C4BA
 with sigma of 0.04
 C20-C18 \\sim C2AA-C5BA
 with sigma of 0.04
 C16-C18 \\sim C4BA-C5BA
 with sigma of 0.04
 C19-C17 \\sim C1AA-C0AA
 with sigma of 0.04
 P1-C21 \\sim P1-C3AA
 with sigma of 0.02
 C21-C26 \\sim C3AA-C4AA
 with sigma of 0.02
 C21-C22 \\sim C3AA-C8AA
 with sigma of 0.02
 C26-C25 \\sim C4AA-C5AA
 with sigma of 0.02
 C23-C24 \\sim C7AA-C6AA
 with sigma of 0.02
 C23-C22 \\sim C7AA-C8AA
 with sigma of 0.02
 C24-C25 \\sim C6AA-C5AA
 with sigma of 0.02
 P1-C26 \\sim P1-C4AA
 with sigma of 0.04
 P1-C22 \\sim P1-C8AA
 with sigma of 0.04
 C21-C23 \\sim C3AA-C7AA
 with sigma of 0.04
 C21-C25 \\sim C3AA-C5AA
 with sigma of 0.04
 C26-C24 \\sim C4AA-C6AA
 with sigma of 0.04
 C26-C22 \\sim C4AA-C8AA
 with sigma of 0.04
 C23-C25 \\sim C7AA-C5AA
 with sigma of 0.04
 C24-C22 \\sim C6AA-C8AA
 with sigma of 0.04
 C50-C49 \\sim C50A-C49A
 with sigma of 0.02
 C50-C45 \\sim C50A-C45A
 with sigma of 0.02
 C49-C48 \\sim C49A-C48A
 with sigma of 0.02
 C48-C47 \\sim C48A-C47A
 with sigma of 0.02
 C47-C46 \\sim C47A-C46A
 with sigma of 0.02
 C46-C45 \\sim C46A-C45A
 with sigma of 0.02
 C50-C48 \\sim C50A-C48A
 with sigma of 0.04
 C50-C46 \\sim C50A-C46A
 with sigma of 0.04
 C49-C47 \\sim C49A-C47A
 with sigma of 0.04
 C49-C45 \\sim C49A-C45A
 with sigma of 0.04
 C48-C46 \\sim C48A-C46A
 with sigma of 0.04
 C47-C45 \\sim C47A-C45A
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C21, C22, C23, C24, C25, C26
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C3AA, C8AA, C7AA, C6AA, C5AA, C4AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.01
 C0, C4BA, C0AA, C5BA, C1AA, C2AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C15, C16, C17, C18, C19, C20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C48A, C47A, C46A, C45A, C50A, C49A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C45, C50, C49, C48, C47, C46
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(C0)=Sof(C4BA)=Sof(H4BA)=Sof(C0AA)=Sof(H0AA)=Sof(C5BA)=Sof(H5BA)=Sof(C1AA)=
 Sof(H1AA)=Sof(C2AA)=Sof(H2AA)=1-FVAR(1)
 Sof(C15)=Sof(C20)=Sof(H20)=Sof(C16)=Sof(H16)=Sof(C18)=Sof(H18)=Sof(C19)=
 Sof(H19)=Sof(C17)=Sof(H17)=FVAR(1)
 Sof(C3AA)=Sof(C4AA)=Sof(H4AA)=Sof(C5AA)=Sof(H5AA)=Sof(C6AA)=Sof(H6AA)=
 Sof(C7AA)=Sof(H7AA)=Sof(C8AA)=Sof(H8AA)=1-FVAR(2)
 Sof(C21)=Sof(C26)=Sof(H26)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C22)=
 Sof(H22)=Sof(C25)=Sof(H25)=FVAR(2)
 Sof(C50A)=Sof(H50A)=Sof(C45A)=Sof(H45A)=Sof(C46A)=Sof(H46A)=Sof(C47A)=
 Sof(H47A)=Sof(C48A)=Sof(H48A)=Sof(C49A)=Sof(H49A)=1-FVAR(3)
 Sof(C50)=Sof(H50)=Sof(C49)=Sof(H49)=Sof(C48)=Sof(H48)=Sof(C47)=Sof(H47)=
 Sof(C46)=Sof(H46)=Sof(C45)=Sof(H45)=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C31(H31), C38(H38), C13(H13), C4(H4), C30(H30), C32(H32), C5(H5), C34(H34),
 C3(H3), C12(H12), C2(H2), C28(H28), C11(H11), C37(H37), C35(H35), C36(H36),
 C20(H20), C10(H10), C42(H42), C16(H16), C29(H29), C54(H54), C43(H43), C52(H52),
  C56(H56), C41(H41), C55(H55), C39(H39), C18(H18), C19(H19), C53(H53),
 C17(H17), C40(H40), C51(H51), C44(H44), C26(H26), C23(H23), C24(H24), C22(H22),
  C25(H25), C4BA(H4BA), C0AA(H0AA), C5BA(H5BA), C1AA(H1AA), C2AA(H2AA),
 C4AA(H4AA), C5AA(H5AA), C6AA(H6AA), C7AA(H7AA), C8AA(H8AA), C50(H50), C49(H49),
  C48(H48), C47(H47), C46(H46), C45(H45), C50A(H50A), C45A(H45A), C46A(H46A),
 C47A(H47A), C48A(H48A), C49A(H49A)
5.b Fitted hexagon refined as free rotating group:
 C50(C49,C48,C47,C46,C45)
;
_shelx_res_checksum              28735
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;